CN108088894A - The apparatus and method that a kind of quick nondestructive differentiates different year grain in storage for years - Google Patents

The apparatus and method that a kind of quick nondestructive differentiates different year grain in storage for years Download PDF

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CN108088894A
CN108088894A CN201611039739.9A CN201611039739A CN108088894A CN 108088894 A CN108088894 A CN 108088894A CN 201611039739 A CN201611039739 A CN 201611039739A CN 108088894 A CN108088894 A CN 108088894A
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gas
grain
years
bottle
storage
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谢园园
李海洋
侯可勇
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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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
    • G01N27/64Investigating 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 using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber

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Abstract

The present invention provides the apparatus and method that a kind of quick nondestructive differentiates different year grain in storage for years, on-line analysis system used includes grain in storage for years sampling apparatus, feeder and gas-detecting device.The on-line analysis is to utilize above-mentioned on-line analysis system, a certain amount of grain in storage for years sample is placed in sampling apparatus, it is heated to certain temperature, release volatile substances contained by sample interior, then provide carrier gas by feeder and carry volatility product outflow sampling apparatus, a part for outflow gas is directly entered gas-detecting device and is analyzed, remaining is discharged as tail gas.The volatility product of various concentration can be obtained by changing the flow velocity of carrier gas and heating temperature, volatility product is directly entered gas-detecting device without concentrating, deriving offline with carrier gas, also without any reagent, it is easy to operate, analysis is accurate, can realize the quick nondestructive discriminating to grain in storage for years.

Description

The apparatus and method that a kind of quick nondestructive differentiates different year grain in storage for years
Technical field
The present invention relates to the apparatus and method that a kind of quick nondestructive differentiates different year grain in storage for years, are exactly specifically to utilize The on-line analysis device heats the grain in storage for years sample of different year, and the sample gas of volatilization is taken out of sample using carrier gas Bottle, finally outflow gas rapidly enters gas-detecting device by gas sampling pipe and carries out ionization analysis, obtains respective characteristic spectrum Figure, so as to fulfill the online purpose for distinguishing different year grain in storage for years.
Background technology
According to relevant regulations, grain in storage for years should not be defined as directly as the grain that grain ration is eaten.It is introduced according to relevant expert, General 3 years of storage time limit of grain in storage for years or more, Aspergillus flavus value is exceeded, and Aspergillus flavus is carcinogen most strong at present, It can still survive at 280 DEG C, carcinogenic required time is most only 24 weeks short, it is thus impossible to which grain in storage for years is eaten directly as grain ration. Whether general detection grain is that the index of grain in storage for years has fatty acid value, and viscosity tastes score value and color and luster smell.Wherein aliphatic acid Value, viscosity and tasting have in score value one reach " ageing " index can regard as grain in storage for years.Fatty acid value is reflection grain The sensitive indexes of food matter judge the important evidence of grain quality quality.For example, China《Paddy storage quality decision rule》 (GB/T 20569-2006) provides that long-grain nonglutinous rice fatty acid value (KOH/ butts)≤30 (mg/100g), which is advisable, to be deposited, 30 (mg/100g) Should not slightly to deposit, fatty acid value > 37 (mg/100g) should not deposit for severe for < fatty acid value≤37 (mg/100g).Japonica rice paddy Fatty acid value (KOH/ butts)≤25 (mg/100g), which is advisable, to be deposited, and 25 (mg/100g) < fatty acid value≤35 (mg/100g) are light Degree should not be deposited, and fatty acid value > 35 (mg/100g) should not deposit for severe.The detection method of grain ageing has guaiacol method, is cured Sore wood phenol-hydroquinone and usage, acid-base indicator method, enzymatic activity method and fatty acid value method etc..Wherein, acid-base indicator method exists Field of fast detection application is most, but this method is identified by color change, and error is larger, and sensitivity is limited, and by Tester's individual difference is affected.Other methods such as fatty acid value method (a kind of Fatty Acid Value In Grain detection reagent, detection method And its application, CN201610431798.4) it needs to use more chemical reagent, manual operation is complicated, and damage is caused to sample It is bad.
A kind of device and new method that are designed to provide quick nondestructive and differentiate different year grain in storage for years of this paper.This method Using sample bottle as the acquisition place of grain in storage for years sample gas, sample is suitably heated, the gaseous product of release enters gas inspection Survey device i.e. using vacuum UV lamp as the positive ion mode time of-flight mass spectrometer of ion source in carry out ionization analysis.This method has Effect solves the deficiency of above-mentioned analysis method, realizes quick nondestructive analysis, is not required any chemical reagents, any pre-concentration, Derivatization or elution step differentiate that different grains in storage for years provide a kind of simple and quick, accurate feasible detection hand for quick nondestructive Section.In addition, the device gas circuit is simple, and it is of low cost, it is easy to operation.
The content of the invention
The object of the present invention is to provide the apparatus and method that a kind of quick nondestructive differentiates different year grain in storage for years.
A kind of quick nondestructive differentiates the device of different year grain in storage for years, it is characterised in that:It is sampled including closed grain in storage for years Device, feeder, carrier gas ingress pipe, carrier gas delivery line and gas-detecting device;
Closed grain in storage for years sampling apparatus includes sample bottle, bottle plug puncture unit, heating module and temperature controller;Sample bottle For the vial of lower end closed, upper end opening, openend is equipped with and can penetrate and flexible seal bottle cap, and bottle is inserted on bottle cap Puncture outfit is filled in, sample bottle outer wall is equipped with heating module, and heating module is connected through temperature controller with external power;
The bottle plug puncture unit has the cylinder of cone point for lower end, in cylinder upper end edge parallel to axial direction A first through hole and a blind hole are offered, in offering second through hole communicated with cylindrical outer on the internal face of blind hole, First through hole is as gas access, and blind hole is as gas vent, and bottle plug puncture unit lower end penetrates bottle cap and enters sample bottle, and first is logical The lower open end in hole and the second through hole are in sample bottle;Gas access and carrier gas ingress pipe are tightly connected, gas vent with Carrier gas delivery line is tightly connected;
The feeder includes carrier gas source of the gas and mass flow controller, and the gas of carrier gas source of the gas is controlled through mass flow Device is passed through by carrier gas ingress pipe in sample bottle, and the gas outlet end of carrier gas ingress pipe is connected with the gas access of bottle plug puncture unit;
The gas vent of bottle plug puncture unit is connected by carrier gas delivery line with the gas sampling pipe of gas-detecting device.
Gas access of the carrier gas through bottle plug puncture unit enters sample bottle, carries the sample gas of grain in storage for years through bottle plug puncture unit Gas vent flows out sample bottle.
The bottle plug puncture unit and sample bottle cap grafting, are sealed by the elasticity of bottle cap itself, prevent from being passed through load The leakage of grain in storage for years sample gas is caused during gas, bottle plug puncture unit can be removed from the bottle cap of sample bottle, and length is adjustable, convenient for containing The grain in storage for years of different quality is put, the tapered distal end of bottle plug puncture unit is located at the top of grain in storage for years sample in sample bottle;Bottle stopper puncture The material of device for can heat safe organic polymer material such as polyether-ether-ketone (PEEK) or stainless steel, prevent heating when its own is released Put chaff interferent impact analysis result;Bottle cap is can heat safe silica gel bottle cap.
Carrier gas source of the gas is not oxygenous inert atmosphere gases (such as nitrogen), and carrier gas ingress pipe is controlled equipped with mass flow Device, carrier gas flux are controllable.
The gas-detecting device is the analytical equipment of direct gas sampling, and the positive ion mode of predominantly gas sampling exists Line mass spectrograph is connected by gas sampling pipe and carrier gas delivery line with sample bottle;Part sampling point to grain in storage for years sample gas Analysis, remaining is discharged as tail gas;
The stainless steel capillary or quartz capillary of gas sampling Guan Weike current limlitings, outside are equipped with electric heater unit (such as electricity Heater strip, electrical heating block and heat tape), certain temperature can be heated to it.
The cavity size of the sample bottle can be adjusted with the dosage of grain in storage for years, ensure that the tapered distal end of bottle plug puncture unit is placed in Above grain in storage for years.
Heating module heating tape, electrical heating block or electric heating wire of resistance for aluminum or stainless steel heat block or centainly, Heating temperature instrument temperature controlled is controllable.
It is operated, is included the following steps using any described device in claim 1-7:
A. the grain in storage for years accurately weighed is put into sample bottle, ensures that grain in storage for years is laid in sample bottle bottom as possible;
B. carrier gas ingress pipe and carrier gas delivery line are tightly connected with bottle plug puncture unit, carrier gas delivery line and gas sampling pipe It is tightly connected, at this time gas there is no to be passed through;
C. bottle plug puncture unit is inserted into sample bottle, the two is tightly connected, the end of bottle plug puncture unit is placed on grain in storage for years Side;
D. using the heating temperature of temperature controller setting heating module, while by gas sampling pipe thermal-stable to required Temperature;
E. mass flow controller is opened immediately, is passed through required flow carrier gas, while using gas-detecting device to outflow Gas on-line sampling obtains the feature spectrogram of the sample gas of grain in storage for years release.
The gas introduction tube and gas eduction tube are organic polymer material pipe or stainless steel tube;
Carrier gas used is not oxygenous inert atmosphere gases, oxidation of the oxygen to grain in storage for years when preventing from heating.
Gas-detecting device is the positive ion mode on-line mass spectroscopy instrument of gas sampling, using vacuum UV lamp ion source to old The Volatile Gas for changing grain carries out ionization analysis, and this method can obtain single characteristic ion peak, and fragment ion is less, is consequently adapted to point The complex component of actual sample volatilization is analysed, their feature spectrogram is obtained, and different year ageing is realized according to its feature spectrogram The quick nondestructive of grain differentiates.
Wherein, for the heating module that heats sample bottle and for heat gas sample feeding pipe electric heater unit can be electricity plus Heated filament, heat tape or electrical heating block.
In view of the complexity for the sample gas component that grain in storage for years sample discharges under heating condition, use vacuum UV lamp for from Component, the photon energy of transmitting is 10.6eV, can realize effectively ionization, and obtained characteristic spectrum to most organic matters Figure is simple, and predominantly the molecular ion of substance, fragment ion are seldom.
Description of the drawings
Fig. 1 is the schematic device that quick nondestructive differentiates different year grain in storage for years:1- sample bottles;2- heating modules;3- bottles Fill in puncture outfit;4- grains in storage for years;5- temperature controllers;6- carrier gas sources of the gas;7- mass flow controllers;8- feeders;9- carrier gas Ingress pipe;10- carrier gas delivery lines;11- gas sampling pipes;12- gas-detecting devices.
Fig. 2 is the feature spectrogram of six kinds of different brands cigarette ashes, and Fig. 3 is the cigarette ash characteristic spectrum of two kinds of scene of fire extractions Figure.
Specific embodiment
First, Fig. 1 is the device that a kind of quick nondestructive differentiates different year grain in storage for years, it is characterised in that:Including closed Grain in storage for years sampling apparatus, feeder 8, carrier gas ingress pipe 9, carrier gas delivery line 10 and gas-detecting device 12;
Closed grain in storage for years sampling apparatus includes sample bottle 1, bottle plug puncture unit 3, heating module 2 and temperature controller 5;Sample Product bottle 1 is lower end closed, the vial of upper end opening, and openend is equipped with and can penetrate and flexible seal bottle cap, is inserted on bottle cap Equipped with bottle plug puncture unit 3,1 outer wall of sample bottle is equipped with heating module 2, and heating module 2 is connected through temperature controller 5 with external power;
The bottle plug puncture unit 3 has the cylinder of cone point for lower end, in cylinder upper end edge parallel to axial side To offering a first through hole and a blind hole, in offered on the internal face of blind hole one communicated with cylindrical outer it is second logical Hole, first through hole is as gas access, and as gas vent, 3 lower end of bottle plug puncture unit penetrates bottle cap and enters sample bottle 1 blind hole, The lower open end of first through hole and the second through hole are in sample bottle 1;Gas access is tightly connected with carrier gas ingress pipe 9, gas Body outlet is tightly connected with carrier gas delivery line 10;
The feeder 8 includes carrier gas source of the gas 6 and mass flow controller 7, and the gas of carrier gas source of the gas 6 is through mass flow Controller 7 is passed through by carrier gas ingress pipe 9 in sample bottle 1, the gas outlet end of carrier gas ingress pipe 9 and the gas of bottle plug puncture unit 3 Entrance is connected;
11 phase of gas sampling pipe that the gas vent of bottle plug puncture unit 3 passes through carrier gas delivery line 10 and gas-detecting device 12 Even.
Gas access of the carrier gas through bottle plug puncture unit 3 enters sample bottle 1, carries the sample gas of grain in storage for years 4 through bottle stopper puncture The gas vent outflow sample bottle 1 of device 3.
The bottle plug puncture unit 3 and 1 bottle cap grafting of sample bottle, are sealed by the elasticity of bottle cap itself, prevent from being passed through The leakage of 4 sample gas of grain in storage for years is caused during carrier gas, bottle plug puncture unit 3 can be removed from the bottle cap of sample bottle 1, and length is adjustable, Convenient for holding the grain in storage for years 4 of different quality, the tapered distal end of bottle plug puncture unit 3 is located at the upper of 4 sample of grain in storage for years in sample bottle 1 Side;The material of bottle plug puncture unit 3 for can heat safe organic polymer material such as polyether-ether-ketone (PEEK) or stainless steel, prevent plus Its own release chaff interferent impact analysis result when hot;Bottle cap is can heat safe silica gel bottle cap.
Carrier gas source of the gas 6 is not oxygenous inert atmosphere gases (such as nitrogen), and carrier gas ingress pipe 9 is equipped with mass flow control Device 7 processed, carrier gas flux is controllable.
The gas-detecting device 12 is the positive ion mode of the analytical equipment of direct gas sampling, predominantly gas sampling On-line mass spectroscopy instrument is connected by gas sampling pipe 11 and carrier gas delivery line 10 with sample bottle 1;To one of 4 sample gas of grain in storage for years Divide sampling analysis, remaining is discharged as tail gas;
Gas sampling pipe 13 for can current limliting stainless steel capillary or quartz capillary, outside be equipped with electric heater unit (such as Electric heating wire, electrical heating block and heat tape), certain temperature can be heated to it.
The cavity size of the sample bottle 1 can be adjusted with the dosage of grain in storage for years 4, ensure the tapered distal end of bottle plug puncture unit 3 It is placed in 4 top of grain in storage for years.
Heating module 2 heating tape, electrical heating block or electrical heating of resistance for aluminum or stainless steel heat block or centainly Silk, heating temperature instrument 5 temperature controlled are controllable.
It is operated, is included the following steps using any described device in claim 1-7:
A. the grain in storage for years 4 accurately weighed is put into sample bottle 1, ensures that grain in storage for years 4 is laid in 1 bottom of sample bottle as possible;
B. carrier gas ingress pipe 9 and carrier gas delivery line 10 are tightly connected with bottle plug puncture unit 3, carrier gas delivery line 10 and gas Sample feeding pipe 11 is tightly connected, and at this time gas there is no to be passed through;
C. bottle plug puncture unit 3 is inserted into sample bottle 1, the two is tightly connected, and the end of bottle plug puncture unit 3 is placed in grain in storage for years 4 tops;
D. the heating temperature of heating module 2 is set using temperature controller 5, while by 11 thermal-stable of gas sampling pipe extremely Required temperature;
E. mass flow controller 7 is opened immediately, is passed through required flow carrier gas, while is utilized 12 convection current of gas-detecting device Outlet on-line sampling obtains the feature spectrogram for the sample gas that grain in storage for years 4 discharges.
The gas introduction tube 9 and gas eduction tube 10 are organic polymer material pipe or stainless steel tube;
Carrier gas used is not oxygenous inert atmosphere gases, oxidation of the oxygen to grain in storage for years when preventing from heating.
Gas-detecting device 12 is the positive ion mode on-line mass spectroscopy instrument of gas sampling, using vacuum UV lamp ion source pair The Volatile Gas of grain in storage for years 4 carries out ionization analysis, and this method can obtain single characteristic ion peak, and fragment ion is less, therefore suitable In the complex component of analysis actual sample volatilization, their feature spectrogram is obtained, and different year is realized according to its feature spectrogram The quick nondestructive of grain in storage for years differentiates.
Wherein, sample bottle uses the Brown Glass Brown glass bottles and jars only of volume about 20ml, and gas sampling pipe uses 250 μm of internal diameter, length about The metal capillary of 1m.Electric heater unit for the heating module for heating hyaloid quality control and for heat gas sample feeding pipe is equal To have the heat tape of certain resistance.In addition, carrier gas ingress pipe uses the polyfluortetraethylene pipe of outer diameter 4mm, gas detection dress The time of-flight mass spectrometer that vacuum UV lamp is used to be ionized for ion source is put, which is designed using orthogonal acceleration, is visited with MCP Device detection is surveyed, a part for the toxic and harmful gas of release enters mass spectrograph by the metal capillary of heating and is analyzed, It is remaining to be discharged as exhaust gas.Ionized region total gas pressure maintains 600Pa or so in experiment.
Embodiment 1
Differentiate the examination of the apparatus and method performance of different year grain in storage for years for a kind of quick nondestructive of the present invention, it is real Test with the ageing rice of four kinds of different years (be respectively 2011,2012,2013 and 2014) as object, using this The sample gas product of their releases of line analysis device on-line analysis, obtains its feature spectrogram, to realize that quick nondestructive differentiates.Setting Flow into the high pure nitrogen of sample bottle is 100mL/min, and grain in storage for years sample quality used is 1.0g.In view of the sample of release The complexity of gas uses vacuum UV lamp as ion source, and the photon energy of transmitting is 10.6eV, and can ionize the overwhelming majority has Machine object, and the feature spectrogram obtained is simple, is mainly the molecular ion of substance, fragment ion is seldom, and ionized region air pressure maintains 600Pa or so.Sample feeding pipe is using 250 μm of internal diameter, the metal capillary of length about 0.5m, and heating unit is heat tape, heating Stablize at 120 DEG C.High pure nitrogen was gathered in the case where no sample adds in before this into line blank test, sampling time 30s.It Afterwards, the grain in storage for years sample of 1.0g is added in, seal bottle cap is buckled, connects gas piping, the heating temperature of sample bottle is set, adds Hot charging is set to aluminum electrical heating block, etc. temperature be upgraded to after 150 DEG C the time of-flight mass spectrometer of positive ion mode to be utilized to carry out immediately Sampling analysis gathers 8 spectrograms to the sample gas of each grain in storage for years.Fig. 2 is the four kinds of different year grains in storage for years obtained at 150 DEG C The feature spectrogram of the sample gas of release, the wherein higher quasi-molecular ions of relative intensity have m/z=19 (for H3O+)、30()、60、 70th, 102,152,162,171,284,308 and 316, intensity is different in the feature spectrogram of four kinds of grains in storage for years.It utilizes SIMCA softwares carry out principal component analysis to above-mentioned data, obtain the principal component analysis figure of Fig. 3.It can be seen that 4 kinds of grains in storage for years The region of each self-forming independence of data point, between each other without infiltration or interference, it was demonstrated that the data obtained using this method can be with Realize that the quick nondestructive of the grain in storage for years sample of different year differentiates.

Claims (10)

1. a kind of quick nondestructive differentiates the device of different year grain in storage for years, it is characterised in that:Including closed grain in storage for years sampling cartridge It puts, feeder (8), carrier gas ingress pipe (9), carrier gas delivery line (10) and gas-detecting device (12);
Closed grain in storage for years sampling apparatus includes sample bottle (1), bottle plug puncture unit (3), heating module (2) and temperature controller (5);Sample bottle (1) is lower end closed, the vial of upper end opening, and openend is equipped with and can penetrate and flexible seal bottle cap, Bottle plug puncture unit (3) is inserted on bottle cap, sample bottle (1) outer wall is equipped with heating module (2), and heating module (2) is controlled through temperature Instrument (5) is connected with external power;
The bottle plug puncture unit (3) has the cylinder of cone point for lower end, in cylinder upper end edge parallel to axial direction A first through hole and a blind hole are offered, in offering second through hole communicated with cylindrical outer on the internal face of blind hole, First through hole is as gas access, and as gas vent, bottle plug puncture unit (3) lower end penetrates bottle cap and enters sample bottle (1) blind hole, The lower open end of first through hole and the second through hole are in sample bottle (1);Gas access connects with carrier gas ingress pipe (9) sealing It connects, gas vent is tightly connected with carrier gas delivery line (10);
The feeder (8) includes carrier gas source of the gas (6) and mass flow controller (7), and the gas of carrier gas source of the gas (6) is through quality Flow controller (7) is passed through by carrier gas ingress pipe (9) in sample bottle (1), and the gas outlet end of carrier gas ingress pipe (9) is worn with bottle stopper The gas access of thorn device (3) is connected;
The gas vent of bottle plug puncture unit (3) passes through carrier gas delivery line (10) and the gas sampling pipe of gas-detecting device (12) (11) it is connected.
2. the apparatus according to claim 1, it is characterised in that:
Gas access of the carrier gas through bottle plug puncture unit (3) enters sample bottle (1), and the sample gas for carrying grain in storage for years (4) is worn through bottle stopper Pierce the gas vent outflow sample bottle (1) of device (3).
3. device according to claim 1 or 2, it is characterised in that:
The bottle plug puncture unit (3) and sample bottle (1) bottle cap grafting, are sealed by the elasticity of bottle cap itself, prevent from being passed through The leakage of grain in storage for years (4) sample gas is caused during carrier gas, bottle plug puncture unit (3) can be removed from the bottle cap of sample bottle (1), and length Adjustable, convenient for holding the grain in storage for years of different quality (4), the tapered distal end of bottle plug puncture unit (3) is located at sample bottle (1) interior grain in storage for years (4) top of sample;The material of bottle plug puncture unit (3) for can heat safe organic polymer material such as polyether-ether-ketone (PEEK) or Stainless steel prevents that its own discharges chaff interferent impact analysis result during heating;Bottle cap is can heat safe silica gel bottle cap.
4. the apparatus according to claim 1, it is characterised in that:
Carrier gas source of the gas (6) is not oxygenous inert atmosphere gases (such as nitrogen), and carrier gas ingress pipe (9) is equipped with mass flow control Device (7) processed, carrier gas flux is controllable.
5. the apparatus according to claim 1, it is characterised in that:
The gas-detecting device (12) is the analytical equipment of direct gas sampling, and the positive ion mode of predominantly gas sampling exists Line mass spectrograph is connected by gas sampling pipe (11) and carrier gas delivery line (10) with sample bottle (1);To grain in storage for years (4) sample gas A part of sampling analysis, remaining as tail gas discharge;
Gas sampling pipe (13) for can current limliting stainless steel capillary or quartz capillary, outside be equipped with electric heater unit (as electricity Heater strip, electrical heating block and heat tape), certain temperature can be heated to it.
6. the apparatus according to claim 1, it is characterised in that:
The cavity size of the sample bottle (1) can be adjusted with the dosage of grain in storage for years (4), ensure the taper end of bottle plug puncture unit (3) End is placed in above grain in storage for years (4).
7. the apparatus according to claim 1, it is characterised in that:
Heating module (2) heating tape, electrical heating block or electric heating wire of resistance for aluminum or stainless steel heat block or centainly, Heating temperature instrument temperature controlled (5) is controllable.
8. a kind of any described devices of claim 1-7 are distinguishing the application of different year grain in storage for years analytic process online, special Sign is:
It is operated, is included the following steps using any described device in claim 1-7:
A. the grain in storage for years accurately weighed (4) is put into sample bottle (1), ensures that grain in storage for years (4) is laid in sample bottle (1) bottom as possible Portion;
B. carrier gas ingress pipe (9) and carrier gas delivery line (10) and bottle plug puncture unit (3) are tightly connected, carrier gas delivery line (10) with Gas sampling pipe (11) is tightly connected, and at this time gas there is no to be passed through;
C. by bottle plug puncture unit (3) insertion sample bottle (1), the two is tightly connected, and the end of bottle plug puncture unit (3) is placed in ageing Above grain (4);
D. using the heating temperature of temperature controller (5) setting heating module (2), while by gas sampling pipe (11) thermal-stable To required temperature;
E. mass flow controller (7) is opened immediately, is passed through required flow carrier gas, while is utilized gas-detecting device (12) convection current Outlet on-line sampling obtains the feature spectrogram for the sample gas that grain in storage for years (4) discharges.
9. application according to claim 8, it is characterised in that:
The gas introduction tube (9) and gas eduction tube (10) are organic polymer material pipe or stainless steel tube;
Carrier gas used is not oxygenous inert atmosphere gases, oxidation of the oxygen to grain in storage for years when preventing from heating.
10. application according to claim 8, it is characterised in that:
Gas-detecting device (12) is the positive ion mode on-line mass spectroscopy instrument of gas sampling, using vacuum UV lamp ion source to old The Volatile Gas for changing grain (4) carries out ionization analysis, and this method can obtain single characteristic ion peak, and fragment ion is less, therefore suitable In the complex component of analysis actual sample volatilization, their feature spectrogram is obtained, and different year is realized according to its feature spectrogram The quick nondestructive of grain in storage for years differentiates.
CN201611039739.9A 2016-11-21 2016-11-21 The apparatus and method that a kind of quick nondestructive differentiates different year grain in storage for years Pending CN108088894A (en)

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CN111257399A (en) * 2018-11-30 2020-06-09 中国科学院大连化学物理研究所 Direct mass spectrum detection device for high-throughput measurement of volatile organic compounds in blood
CN111474020A (en) * 2019-01-24 2020-07-31 应急管理部沈阳消防研究所 Pretreatment device and method for component analysis of large-batch ash samples

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Application publication date: 20180529