CN107153014A - A kind of detection method of papermaking-method reconstituted tobaccos material breath composition - Google Patents

A kind of detection method of papermaking-method reconstituted tobaccos material breath composition Download PDF

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Publication number
CN107153014A
CN107153014A CN201610118551.7A CN201610118551A CN107153014A CN 107153014 A CN107153014 A CN 107153014A CN 201610118551 A CN201610118551 A CN 201610118551A CN 107153014 A CN107153014 A CN 107153014A
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CN
China
Prior art keywords
papermaking
reconstituted tobaccos
breath composition
sampling pipe
breath
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201610118551.7A
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Chinese (zh)
Inventor
严新龙
张钰
张登
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANGHAI TOBACCO GROUP TAICANG HAIYAN TOBACCO RECONSTITUTED TOBACCO CO Ltd
Shanghai Tobacco Group Co Ltd
Original Assignee
SHANGHAI TOBACCO GROUP TAICANG HAIYAN TOBACCO RECONSTITUTED TOBACCO CO Ltd
Shanghai Tobacco Group Co Ltd
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Application filed by SHANGHAI TOBACCO GROUP TAICANG HAIYAN TOBACCO RECONSTITUTED TOBACCO CO Ltd, Shanghai Tobacco Group Co Ltd filed Critical SHANGHAI TOBACCO GROUP TAICANG HAIYAN TOBACCO RECONSTITUTED TOBACCO CO Ltd
Priority to CN201610118551.7A priority Critical patent/CN107153014A/en
Publication of CN107153014A publication Critical patent/CN107153014A/en
Pending legal-status Critical Current

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Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/14Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • G01N1/2202Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025Gas chromatography

Abstract

The present invention provides a kind of detection method of papermaking-method reconstituted tobaccos material breath composition, the Volatile Organic Components around reconstituted tobacco material are enriched in adsorption sampling pipe by air sampler, then thermal desorption-gas chromatography-mass spectrum technology is utilized, the breath composition that material is volatilized in papermaking-method reconstituted tobaccos finished product and production process is determined.A kind of detection method for papermaking-method reconstituted tobaccos material breath composition that the present invention is provided, with it is easy to operation, quick, accurate the features such as, the changing rule of breath composition especially smell component can be effectively grasped, important technical support is provided for the cleaning anticorrosive work of production line.

Description

A kind of detection method of papermaking-method reconstituted tobaccos material breath composition
Technical field
The invention belongs to the technical field of papermaking-method reconstituted tobaccos, it is related to a kind of detection of papermaking-method reconstituted tobaccos material breath composition Method.
Background technology
Papermaking-method reconstituted tobaccos are to want former based on the offal discarded during production of cigarettes, the low-grade hypo-tobacco leaf of offal and part Material, is equipped with a small amount of plus fiber, the tobacco leaf product for being processed restructuring with reference to pulping and papermaking process technology and obtaining.Its papermaking Method reconstituted tobacco technique can not only reduce production of cigarettes cost, can also improve product quality, can especially significantly reduce in cigarette The content of tar.
At present, papermaking-method reconstituted tobaccos technique include extraction, slurrying, manufacture paper with pulp, coating fluid processed, cutting packing etc. process. Generally raw material is extracted by solvent of water in papermaking-method reconstituted tobaccos production, in whole process, process materials (including extraction Liquid, plain boiled water, slurry etc.) belong to moisture height, the material of complex chemical composition, under hot and humid environment, during storage Between it is long, it may occur that go mouldy, the phenomenon such as corruption, be different from the special dulcet peculiar smell of tobacco while producing, this pacifies to product quality Bring threat entirely.
It is the clear of production scene therefore, it is necessary to study the breath changing rule in papermaking-method reconstituted tobaccos production process The work such as clean anti-corrosion provide technical support, so as to ensure the safe mass of product.This is a kind of for perishable material firstly the need of proposing The detection method of breath, however, for the research open report nearly no at present of breath in papermaking-method reconstituted tobaccos process materials.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of papermaking-method reconstituted tobaccos material breath into The detection method divided, understands the changing rule of breath during produced on-site, and the cleaning anticorrosive work for scene provides technical support, So as to ensure the safe mass of product.
In order to achieve the above objects and other related objects, the present invention provides a kind of detection of papermaking-method reconstituted tobaccos material breath composition Method, comprises the following steps:
It is preferred that the papermaking-method reconstituted tobaccos material breath composition includes the process in the raw material of papermaking-method reconstituted tobaccos, production Volatile organic matter around material (including extract, slurry, plain boiled water etc.) and finished product.Due to papermaking-method reconstituted tobaccos Formula is different, and the process materials added in production process are different, so that the finished product obtained is also different so that papermaking-method reconstituted tobaccos The breath composition that material is volatilized is also different.
1) papermaking-method reconstituted tobaccos material breath composition is gathered using harvester;
It is preferred that the harvester collection papermaking-method reconstituted tobaccos material breath composition, including harvester collection paper process is again Make process materials breath composition in leaf tobacco production and harvester collection papermaking-method reconstituted tobaccos raw material (offal, tobacco chippings and Offal) or finished product materials breath composition.
Preferably, the process materials breath composition in the harvester collection papermaking-method reconstituted tobaccos production, comprises the following steps:
A) harvester includes connecting tube, adsorption sampling pipe and gas collecting pump, by one end of adsorption sampling pipe It is connected through connecting tube with the container containing the process materials in papermaking-method reconstituted tobaccos production, while will absorption The other end of sampling pipe is connected with gas collecting pump, constitutes harvester;
It is highly preferred that one end of the adsorption sampling pipe and connecting tube airtight connection, the other end and gas of the adsorption sampling pipe Gather pump airtight connection.
B) setting sampling time and sampling flow, start gas collecting pump and are acquired;
It is highly preferred that the gas collecting pump is air sampler.
It is highly preferred that the acquisition condition of the gas collecting pump is:Gas flow acquisition range:0-1.00L/min;Sampling flow: 0.10-0.80L/min;Sampling time:5-60min.
It is highly preferred that the acquisition condition of the gas collecting pump is:Gas flow acquisition range:0-1.00L/min;Sampling flow: 0.10-0.50L/min;Sampling time:10-30min.
Above-mentioned sampling time and sampling flow, within the adsorption capacity allowed band of adsorption tube, and gas chromatography-mass spectrography The chromatogram peak type that method is determined preferably, response it is preferable.
C) the gas collecting pump is aspirated the container of the process materials in being produced containing papermaking-method reconstituted tobaccos by sampling flow In papermaking-method reconstituted tobaccos production in process materials breath composition, breath composition is by being connected on pump During adsorption sampling pipe, the adsorbent absorption filled in adsorbed sampling pipe;
D adsorption sampling pipe two ends are sealed with sealing copper cap after) sampling terminates, it is to be measured.
Preferably, the harvester collection papermaking-method reconstituted tobaccos raw material (offal, tobacco chippings and offal) or finished product materials Breath composition, comprises the following steps:
A) harvester includes adsorption sampling pipe, and adsorption sampling pipe is placed directly in containing papermaking-method reconstituted tobaccos In raw material or the container of finished product materials;
B) the adsorption sampling pipe is in the container containing papermaking-method reconstituted tobaccos raw material or finished product materials, Static Adsorption papermaking Method reconstituted tobacco raw material or finished product materials breath composition;
It is highly preferred that the time of the Static Adsorption is 1~20h.
C) adsorption sampling pipe two ends are sealed with sealing copper cap after sampling terminates, it is to be measured.
It is highly preferred that above-mentioned adsorption sampling pipe is composite filled type adsorption sampling pipe, the adsorbent of inside filling for Tenax TA or Bis- sections of Tenax TA and Graphitised Carbon Black are combined.
It is highly preferred that the two ends of above-mentioned adsorption sampling pipe are formulated with sealing copper cap.
It is highly preferred that above-mentioned adsorption sampling pipe will carry out aging before collection breath composition.
It is further preferred that the aging is carried out using ageing device.
It is further preferred that the aging condition is:Ageing gas:Nitrogen, purity is 99.999%;Ageing gas pressure: 15-25psi;Aging temperature:280-320℃;Ageing time:20-40min.
Most preferably, the aging condition is:Ageing gas:Nitrogen, purity is 99.999%;Ageing gas pressure:20psi; Aging temperature:300-320℃;Ageing time:30min.
It is further preferred that the adsorption sampling pipe is after aging, adsorption sampling pipe two ends are sealed with sealing copper cap, it is standby.
2) by step 1) collection breath composition, carry out thermal desorption;
It is preferred that the thermal desorption is carried out in thermal desorption instrument.I.e. using thermal desorption instrument to the breath adsorbed in adsorption sampling pipe into Divide and carry out thermal desorption.
Preferably, the thermal desorption instrument is connected by the transmission line of a heating and thermal insulation with gas chromatograph-mass spectrometer (GC-MS).
It is preferred that the condition of the thermal desorption is:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:1~4min; One-level is desorbed:Temperature is 220~300 DEG C, and the time is 5~15min, and desorption flow is 40~60ml/min;Import is not shunted;It is cold Hydrazine is in 0~-30 DEG C of enrichments;Two grades of desorptions:Temperature is 250~320 DEG C, and the time is 2~4min;Desorption flow is 15~25ml/min, Outlet manifold, bypass flow is 15~25ml/min.
Preferably, the condition of the thermal desorption is:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:1~3min; One-level is desorbed:Temperature is 240~300 DEG C, and the time is 5~15min, and desorption flow is 50ml/min;Import is not shunted;Cold hydrazine In -10~-30 DEG C of enrichments;Two grades of desorptions:Temperature is 260~320 DEG C, and the time is 3min;Desorption flow is 20ml/min, outlet Shunting, bypass flow is 20ml/min.
3) will be through step 2) breath composition after thermal desorption, it is measured using gas chromatography-mass spectrometry (GC-MS).
It is preferred that the GC conditions are:Chromatographic column:DB-waxlter capillary columns (60m × 0.32mm i.d. × 1.8 μm df);Thermal desorption and gas-chromatography transmission line temperature:180℃;Carrier gas:High-purity helium, carrier gas purity >=99.999%;Flow velocity: 0.8-1.2mL/min;Splitless injecting samples;Heating schedule:40 DEG C of initial temperature, 220 DEG C, guarantor are risen to 5 DEG C/min speed 5min is held, the bulk analysis time is 41min.
It is preferred that the Mass Spectrometry Conditions are:Makings coffret temperature:250℃;Ion source temperature:230℃;Level Four bar temperature Degree:150℃;Solvent delay:0.5min;Ionization mode:EI sources;Ionizing energy:70eV;Scan mode:Full scan (Scan); Mass scan range m/z:29~250amu.
It is preferred that the gas chromatography-mass spectrometry uses NIST standard spectrums storehouse to papermaking-method reconstituted tobaccos material breath composition Carry out library searching qualitative.
Preferably, the NIST standard spectrums storehouse is that NIST11.L composes storehouse.
Preferably, the NIST standard spectrums storehouse selects matching degree >=80 to breath composition basis for estimation.
As described above, a kind of detection method of papermaking-method reconstituted tobaccos material breath composition of the present invention, will by air sampler Volatile Organic Components around reconstituted tobacco material are enriched in adsorption sampling pipe, then utilize thermal desorption-gas-chromatography-matter GC-MS is composed, the breath composition that material is volatilized in papermaking-method reconstituted tobaccos finished product and production process is determined.There is provided in the present invention A kind of papermaking-method reconstituted tobaccos material breath composition detection method, with it is easy to operation, quick, accurate the features such as. It is quick, efficient that it analyzes process;Acquired results are more accurate.It can be detected in papermaking-method reconstituted tobaccos material and distinguished by the present invention It is the clear of production line so as to grasp the changing rule of breath composition especially smell component in the smell component of the special breath of tobacco Clean anticorrosive work provides important technical support.
Brief description of the drawings
Fig. 1 is shown as the full scan gas-chromatography of process materials (tobacco slurry) breath composition in papermaking-method reconstituted tobaccos production Figure.
Fig. 2 is shown as causing process materials (tobacco slurry) the smell component propionic acid difference storage in papermaking-method reconstituted tobaccos production Selection chromatography of ions figure under time.
Embodiment
The present invention is expanded on further with reference to specific embodiment, it should be appreciated that these embodiments be merely to illustrate the present invention and without In limiting the scope of the invention.
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be as disclosed by this specification Content understand easily the present invention other advantages and effect.The present invention can also add by way of a different and different embodiment To implement or apply, the various details in this specification can also be based on different viewpoints and application, in the essence without departing from the present invention God is lower to carry out various modifications or alterations.
Material, reagent and instrument that following examples are used:
Papermaking-method reconstituted tobaccos material (is selected from Shanghai Tobacco Group Taicang Haiyan Tobacco Reconstituted Tobacco Co., Ltd.);TC-20 type agings Instrument (Markes companies of Britain);TMP-1500A types air sampler (Yancheng Ke Bo Electron equipment Co., Ltd);TD-100 Type thermal desorption instrument (Markes companies of Britain);GC 7890A/MS 5975C Gc/ms Analysers (U.S. Agilent Company);Adsorbent:(Britain Markes is public by Tenax TA, Graphitised Carbon Black, Carbonised Molecular Department.
Embodiment 1
1st, sample pre-treatments
The adsorption sampling pipe for filling adsorbent is subjected to aging on ageing device, under the nitrogen atmosphere of purity >=99.999%, kept Nitrogen pressure 15-25psi, the aging 20-40min at 280-320 DEG C.The effective copper cap sealing both ends of the complete adsorption sampling of aging, it is standby With.Adsorption sampling pipe be composite filled type adsorption sampling pipe, inside filling adsorbent for Tenax TA or Tenax TA with Bis- sections of Graphitised Carbon Black are combined.
Then, when gather papermaking-method reconstituted tobaccos production in process materials breath composition when, by one end of connecting tube be placed in containing In the container of process materials in papermaking-method reconstituted tobaccos production, and the top of material is located at, after other end connection aging One end of the adsorption sampling pipe of adsorbent is filled, the other end of adsorption sampling pipe is connected with gas collecting pump seal.Gas collecting pump With 0.10-0.80L/min flow, preferably 0.10-0.50L/min, the breath composition around material is evacuated in adsorption sampling pipe, The adsorption sampling time is that 5-60min is preferably 10-30min.Adsorption sampling pipe two ends are sealed with sealing copper cap after the completion of absorption, It is standby.
When gathering papermaking-method reconstituted tobaccos raw material (offal, tobacco chippings and offal) or finished product materials breath composition, it will adsorb Sampling pipe is placed directly in the container containing papermaking-method reconstituted tobaccos raw material or finished product materials, Static Adsorption papermaking-method reconstituted tobaccos Raw material or finished product materials breath composition, the time of Static Adsorption is 1~20h, and sealing copper cap is used after the completion of absorption by adsorption sampling pipe Two ends are sealed, standby.
2nd, thermal desorption and GC-MS are determined
The breath composition adsorbed in adsorption sampling pipe is subjected to thermal desorption by thermal desorption instrument, and passes through gas chromatograph-mass spectrometer (GC-MS) Breath composition after thermal desorption is measured.Transmission line and gas chromatography-mass spectrometry that thermal desorption instrument passes through a heating and thermal insulation It is connected with instrument.
Wherein, the condition of the thermal desorption is:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:1~4min; One-level is desorbed:Temperature is 220~300 DEG C, and the time is 5~15min, and desorption flow is 40~60ml/min;Import is not shunted;It is cold Hydrazine is in 0~-30 DEG C of enrichments;Two grades of desorptions:Temperature is 250~320 DEG C, and the time is 2~4min;Desorption flow is 15~25ml/min, Outlet manifold, bypass flow is 15~25ml/min.
It is preferred that the condition of thermal desorption be:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:1~3min;One Level desorption:Temperature is 240~300 DEG C, and the time is 5~15min, and desorption flow is 50ml/min;Import is not shunted;Cold hydrazine is -10~-30 DEG C enrichment;Two grades of desorptions:Temperature is 260~320 DEG C, and the time is 3min;Desorption flow is 20ml/min, and outlet manifold divides Stream flow is 20ml/min.
The GC conditions are:Chromatographic column:DB-waxlter capillary columns (60m × 0.32mm i.d. × 1.8 μm df);Heat Desorption and gas-chromatography transmission line temperature:180℃;Carrier gas:High-purity helium, carrier gas purity >=99.999%;Flow velocity:0.8-1.2mL /min;Splitless injecting samples;Heating schedule:40 DEG C of initial temperature, 220 DEG C are risen to 5 DEG C/min speed, keep 5min, The bulk analysis time is 41min.
The Mass Spectrometry Conditions are:Makings coffret temperature:250℃;Ion source temperature:230℃;Level Four bar temperature:150 ℃;Solvent delay:0.5min;Ionization mode:EI sources;Ionizing energy:70eV;Scan mode:Full scan (Scan);Matter Measure scanning range m/z:29~250amu.
The testing result of papermaking-method reconstituted tobaccos material breath composition is qualitative using the progress retrieval matching of NIST11.L standard spectrums storehouse, right Breath composition basis for estimation selects matching degree >=80, so as to obtain the qualitative detection result of papermaking-method reconstituted tobaccos material breath composition.
Embodiment 2
1st, sample pre-treatments
The adsorption sampling pipe for filling adsorbent is subjected to aging on TC-20 type ageing devices, in the blanket of nitrogen of purity >=99.999% Under enclosing, nitrogen pressure 20psi, the aging 30min at 320 DEG C are kept.The effective copper cap sealing both ends of the complete adsorption sampling of aging, It is standby.Adsorption sampling pipe is filled-type adsorption sampling pipe, and the adsorbent of inside filling is Tenax TA.
Then, the container for the process materials (tobacco slurry) one end of connecting tube being placed in being produced containing papermaking-method reconstituted tobaccos It is interior, and the top of tobacco slurry is located at, one end of the adsorption sampling pipe of the filling adsorbent after other end connection aging is inhaled The other end of attached sampling pipe is tightly connected with TMP-1500A type air samplers.TMP-1500A types air sampler with 0.20L/min flow, the breath composition around material is evacuated in adsorption sampling pipe, and the adsorption sampling time is 20min.Absorption After the completion of with sealing copper cap by adsorption sampling pipe two ends seal, it is standby.
2nd, thermal desorption and GC-MS are determined
The breath composition adsorbed in adsorption sampling pipe is subjected to thermal desorption by TD-100 type thermal desorptions instrument, and passes through GC 7890A / MS 5975C gas chromatograph-mass spectrometer (GC-MS)s are measured to the breath composition after thermal desorption.TD-100 type thermal desorption instrument passes through The transmission line of a piece heating and thermal insulation is connected with GC 7890A/MS 5975C gas chromatograph-mass spectrometer (GC-MS)s.
Wherein, the condition of the thermal desorption is:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:3min; One-level is desorbed:Temperature is 280 DEG C, and the time is 10min, and desorption flow is 50ml/min;Import is not shunted;Cold hydrazine is at -20 DEG C Enrichment;Two grades of desorptions:Temperature is 280 DEG C, and the time is 3min, and desorption flow is 20ml/min;Outlet manifold, bypass flow For 20ml/min.
The GC conditions are:Chromatographic column:DB-waxlter capillary columns (60m × 0.32mm i.d. × 1.8 μm df);Heat Desorption and gas-chromatography transmission line temperature:180℃;Carrier gas:High-purity helium, carrier gas purity >=99.999%;Flow velocity:1.0mL/min; Splitless injecting samples;Heating schedule:40 DEG C of initial temperature, 220 DEG C are risen to 5 DEG C/min speed, keep 5min, bulk analysis Time is 41min.
The Mass Spectrometry Conditions are:Makings coffret temperature:250℃;Ion source temperature:230℃;Level Four bar temperature:150 DEG C solvent delay:0.5min;Ionization mode:EI sources;Ionizing energy:70eV;Scan mode:Full scan (Scan);Quality Scanning range m/z:29~250amu.
The testing result of process materials breath composition in papermaking-method reconstituted tobaccos production is examined using NIST11.L standard spectrums storehouse Rope matching is qualitative, and matching degree >=80 are selected to breath composition basis for estimation, so as to obtain the process thing in papermaking-method reconstituted tobaccos production Expect the qualitative detection result of (tobacco slurry), be shown in Table 1.As shown in Table 1, the process materials in papermaking-method reconstituted tobaccos production (tobacco slurry) breath composition, when matching degree >=80, detects 50 kinds of breath compositions altogether.Papermaking-method reconstituted tobaccos life simultaneously The full scan gas chromatogram of process materials (tobacco slurry) breath composition in production is shown in Fig. 1.
Process materials breath composition analysis result in the production of the papermaking-method reconstituted tobaccos of table 1
Embodiment 3
1st, sample pre-treatments
The adsorption sampling pipe for filling adsorbent is subjected to aging on TC-20 type ageing devices, in the blanket of nitrogen of purity >=99.999% Under enclosing, nitrogen pressure 20psi, the aging 30min at 310 DEG C are kept.The effective copper cap sealing both ends of the complete adsorption sampling of aging, It is standby.Adsorption sampling pipe is filled-type adsorption sampling pipe, and the adsorbent of inside filling is Tenax TA and Graphitised Carbon Bis- sections of Black is combined.
Then, the adsorption sampling pipe after aging is placed in the container containing papermaking-method reconstituted tobaccos raw material offal, Static Adsorption 12h. Adsorption sampling pipe two ends are sealed with sealing copper cap after the completion of absorption, it is standby.
2nd, thermal desorption and GC-MS are determined
The breath composition adsorbed in adsorption sampling pipe is subjected to thermal desorption by TD-100 type thermal desorptions instrument, and passes through GC 7890A / MS 5975C gas chromatograph-mass spectrometer (GC-MS)s are measured to the breath composition after thermal desorption.TD-100 type thermal desorption instrument passes through The transmission line of a piece heating and thermal insulation is connected with GC 7890A/MS 5975C gas chromatograph-mass spectrometer (GC-MS)s.
Wherein, the condition of the thermal desorption is:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:3min; One-level is desorbed:Temperature is 270 DEG C, and the time is 9min, and desorption flow is 50ml/min;Import is not shunted;Cold hydrazine is in -15 DEG C of richnesses Collection;Two grades of desorptions:Temperature is 300 DEG C, and the time is 3min, and desorption flow is 20ml/min;Outlet manifold, bypass flow is 20ml/min。
The GC conditions are:Chromatographic column:DB-waxlter capillary columns (60m × 0.32mm i.d. × 1.8 μm df);Heat Desorption and gas-chromatography transmission line temperature:180℃;Carrier gas:High-purity helium, carrier gas purity >=99.999%;Flow velocity:1.1mL/min; Splitless injecting samples;Heating schedule:40 DEG C of initial temperature, 220 DEG C are risen to 5 DEG C/min speed, keep 5min, bulk analysis Time is 41min.
The Mass Spectrometry Conditions are:Makings coffret temperature:250℃;Ion source temperature:230℃;Level Four bar temperature:150 ℃;Solvent delay:0.5min;Ionization mode:EI sources;Ionizing energy:70eV;Scan mode:Full scan (Scan);Matter Measure scanning range m/z:29~250amu.
It is fixed that the testing result of papermaking-method reconstituted tobaccos feed product breath composition carries out retrieval matching using NIST11.L standard spectrums storehouse Property, matching degree >=80 are selected breath composition basis for estimation, so as to obtain determining for the breath composition of papermaking-method reconstituted tobaccos raw material offal Property testing result, concrete outcome is shown in Table 2.
The papermaking-method reconstituted tobaccos feed product breath composition analysis result of table 2
Sequence number Retention time (is divided) Peak area (Ab*s) Qualitative matching degree Components Name
1 4.81 2109594 81 N-hexane
2 6.024 8739178 87 2 methyl propanal
3 7.144 1201837 53 2- butanone
4 7.35 4298393 87 2 methyl butyraldehyde
5 7.422 16111939 93 3- methylbutyraldehyds
6 8.49 33210554 72 2,3- diacetyl
7 9.953 3566089 93 Toluene
8 10.906 7299688 90 Hexanal
9 12.134 2131481 91 Ethylbenzene
10 12.521 2679418 97 Paraxylene
11 13.367 3828652 91 1- ethyl methyl benzenes
12 13.696 3841051 94 Pyrroles
13 13.743 1503470 93 Ortho-xylene
14 14.023 2271429 78 3- methyl butanols
15 15.201 1544406 72 Amylalcohol
16 15.506 2233285 98 Tetrahydrochysene dicyclopentadiene
17 15.75 760868 93 Styrene
18 16.654 27931989 86 3-Hydroxybutanone
19 17.126 17226686 72 1- hydroxyls, 2- acetone
20 17.823 1736699 87 Methyl heptenone
21 20.855 1072148739 91 Acetic acid
22 21.44 7994899 91 Furfural
23 22.519 1292763 90 Acetyl furan
24 22.645 7306874 83 Formic acid
25 23.112 12463490 95 Phenylacetaldehyde
26 23.194 16892432 91 Propionic acid
27 23.95 8497111 90 The butanol of 2,3- bis-
28 24.252 915726 81 5 methyl furfural
29 24.691 2676450 76 The diketone of 4- cyclopentene -1,3
30 25.949 30459797 91 Butyrolactone
31 26.094 6211604 97 Furfuryl alcohol
32 26.328 6554265 72 3 Methylbutanoic acid
33 27.651 1713794 91 Solanone
34 31.122 5433781 96 Phenmethylol
35 33.223 4356200 92 Acetyl pyrrole
36 36.828 1812754 93 Hexadecane
Embodiment 4
1st, sample pre-treatments
The adsorption sampling pipe for filling adsorbent is subjected to aging on TC-20 type ageing devices, in the blanket of nitrogen of purity >=99.999% Under enclosing, nitrogen pressure 20psi, the aging 30min at 300 DEG C are kept.The effective copper cap sealing both ends of the complete adsorption sampling of aging, It is standby.Adsorption sampling pipe is filled-type adsorption sampling pipe, and the adsorbent of inside filling is Tenax TA.
Then, the container for the process materials (tobacco slurry) one end of connecting tube being placed in being produced containing papermaking-method reconstituted tobaccos It is interior, and the top of tobacco slurry is located at, one end of the adsorption sampling pipe of the filling adsorbent after other end connection aging is inhaled The other end of attached sampling pipe is tightly connected with TMP-1500A type air samplers.TMP-1500A types air sampler with 0.15L/min flow, the breath composition around material is evacuated in adsorption sampling pipe, and the adsorption sampling time is 30min.Absorption After the completion of with sealing copper cap by adsorption sampling pipe two ends seal, it is standby.
2nd, thermal desorption and GC-MS are determined
The breath composition adsorbed in adsorption sampling pipe is subjected to thermal desorption by TD-100 type thermal desorptions instrument, and passes through GC 7890A / MS 5975C gas chromatograph-mass spectrometer (GC-MS)s are measured to the breath composition after thermal desorption.TD-100 type thermal desorption instrument passes through The transmission line of a piece heating and thermal insulation is connected with GC 7890A/MS 5975C gas chromatograph-mass spectrometer (GC-MS)s.
Wherein, the condition of the thermal desorption is:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:3min; One-level is desorbed:Temperature is 260 DEG C, and the time is 8min, and desorption flow is 50ml/min;Import is not shunted;Cold hydrazine is in -10 DEG C of richnesses Collection;Two grades of desorptions:Temperature is 280 DEG C, and the time is 3min, and desorption flow is 20ml/min;Outlet manifold, bypass flow: 20ml/min。
The GC conditions are:Chromatographic column:DB-waxlter capillary columns (60m × 0.32mm i.d. × 1.8 μm df);Heat Desorption and gas-chromatography transmission line temperature:180℃;Carrier gas:High-purity helium, carrier gas purity >=99.999%;Flow velocity:1.0mL/min; Splitless injecting samples;Heating schedule:40 DEG C of initial temperature, 220 DEG C are risen to 5 DEG C/min speed, keep 5min, bulk analysis Time is 41min.
The Mass Spectrometry Conditions are:Makings coffret temperature:250℃;Ion source temperature:230℃;Level Four bar temperature:150 ℃;Solvent delay:0.5min;Ionization mode:EI sources;Ionizing energy:70eV;Scan mode:Full scan (Scan);Matter Measure scanning range m/z:29~250amu.
The testing result of process materials (tobacco slurry) breath composition in papermaking-method reconstituted tobaccos production uses NIST11.L standards Compose storehouse progress retrieval matching qualitative, matching degree >=80 are selected to breath composition basis for estimation, so as to obtain papermaking-method reconstituted tobaccos production In process materials (tobacco slurry) breath composition qualitative detection result.
Embodiment 5
Using testing conditions same as Example 2, adsorbed, inhaled by the adsorption sampling pipe containing different filling adsorbents Contained filling adsorbent is respectively Tenax TA, Tenax TA and bis- sections of Graphitised Carbon Black multiple in attached sampling pipe Conjunction, Tenax TA, Graphitised Carbon Black, tri- sections of Carbonised Molecular are combined.Testing result such as table 3.
The influence of adsorption sampling pipe of the table 3 containing different filling adsorbents
As shown in Table 3, moisture is high in the process materials (tobacco slurry) in being produced due to papermaking-method reconstituted tobaccos, relatively closes Suitable adsorption tube should not contain carbonised Molecular (carbon molecular sieve) composition, otherwise because carbon molecular sieve is easily adsorbed Hydrone, can influence the accuracy and authenticity of testing result.
Embodiment 6
The testing result of process materials (tobacco slurry) breath composition in the papermaking-method reconstituted tobaccos production in embodiment 4 is adopted Retrieval matching is carried out with NIST11.L standard spectrums storehouse qualitative.For reconstituted tobacco material can be caused to produce the property material of peculiar smell:Third Sour composition (characteristic ion is 74) has carried out selection ion analysis.As a result understand, when production line is normally run, from scene taking-up Process materials (tobacco slurry) in do not detect propionic acid composition.
Meanwhile, using testing conditions same as Example 4, in the papermaking-method reconstituted tobaccos production of different resting periods Process materials (tobacco slurry) are measured, on the basis of detection full scan chromatogram, using characteristic ion as 74, extract choosing Chromatography of ions figure is selected, so as to obtain the peak area of propionic acid, the influence of different resting periods is as shown in table 4.Meanwhile, in production Process materials (tobacco slurry) selection chromatography of ions figure of propionic acid composition within the different resting periods is shown in Fig. 2.
The different resting period influences of table 4
The slurry resting period/h Propionic acid peak area
0 0
2 4.23×106
8 6.48×107
As shown in Table 4, when the normal operation of production, the process materials (tobacco slurry) in online papermaking-method reconstituted tobaccos production are taken Detected, do not include the propionic acid composition that reconstituted tobacco material can be caused to produce peculiar smell in its 50 kinds of breath composition detected, i.e., Propionic acid composition is not detected.But as the resting period extends, then to the process materials (tobacco pulp in papermaking-method reconstituted tobaccos production Material) detected occur propionic acid composition in testing result, its peak area is dramatically increased, and is illustrated that propionic acid content is more and more, is made Process materials (tobacco slurry) in the production of paper method reconstituted tobacco show obvious tart flavour.It can be seen that, pass through method in the present invention The smell component of the special breath of tobacco can be gone out in papermaking-method reconstituted tobaccos material to be different from effective detection, so as to grasp breath composition The especially changing rule of smell component, the cleaning anticorrosive work to production line is significant.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any to be familiar with this skill The personage of art all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Therefore, such as Those of ordinary skill in the art without departing from disclosed spirit with completed under technological thought all etc. Modifications and changes are imitated, should be covered by the claim of the present invention.

Claims (11)

1. a kind of detection method of papermaking-method reconstituted tobaccos material breath composition, comprises the following steps:
1) papermaking-method reconstituted tobaccos material breath composition is gathered using harvester;
2) by step 1) collection breath composition, carry out thermal desorption;
3) will be through step 2) breath composition after thermal desorption, it is measured using gas chromatography-mass spectrometry.
2. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 1, it is characterised in that step 1) In, the harvester gathers papermaking-method reconstituted tobaccos material breath composition, including harvester collection papermaking-method reconstituted tobaccos Process materials breath composition, harvester collection papermaking-method reconstituted tobaccos raw material or finished product materials breath composition in production.
3. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 2, it is characterised in that the collection Process materials breath composition in device collection papermaking-method reconstituted tobaccos production, comprises the following steps:
A) harvester includes connecting tube, adsorption sampling pipe and gas collecting pump, by one end of adsorption sampling pipe through connection Pipe is connected with containing the container of process materials in papermaking-method reconstituted tobaccos production, while by the another of adsorption sampling pipe End is connected with gas collecting pump, constitutes harvester;
B) setting sampling time and sampling flow, start gas collecting pump and are acquired;
C) the gas collecting pump is aspirated by sampling flow in the container of the process materials in being produced containing papermaking-method reconstituted tobaccos Process materials breath composition in papermaking-method reconstituted tobaccos production, breath composition passes through the adsorption sampling pipe that is connected on pump When, it is adsorbed the adsorbent absorption filled in sampling pipe;
D adsorption sampling pipe two ends are sealed with sealing copper cap after) sampling terminates, it is to be measured.
4. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 3, it is characterised in that the gas Collection pump acquisition condition be:Gas flow acquisition range:0-1.00L/min;Sampling flow:0.10-0.80L/min;Adopt The sample time:5-60min.
5. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 2, it is characterised in that the collection Device gathers papermaking-method reconstituted tobaccos raw material or finished product materials breath composition, comprises the following steps:
A) harvester includes adsorption sampling pipe, and adsorption sampling pipe is placed directly in containing papermaking-method reconstituted tobaccos raw material Or in the container of finished product materials;
B) the adsorption sampling pipe is in the container containing papermaking-method reconstituted tobaccos raw material or finished product materials, and Static Adsorption paper process is again Make raw tobacco material or finished product materials breath composition;
C) adsorption sampling pipe two ends are sealed with sealing copper cap after sampling terminates, it is to be measured.
6. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 5, it is characterised in that the static state The time of absorption is 1~20h.
7. according to the detection method of any described papermaking-method reconstituted tobaccos material breath composition of claim 3 or 5, it is characterised in that The adsorption sampling pipe be composite filled type adsorption sampling pipe, inside filling adsorbent for Tenax TA or Tenax TA with Bis- sections of Graphitised Carbon Black are combined.
8. according to the detection method of any described papermaking-method reconstituted tobaccos material breath composition of claim 3 or 5, it is characterised in that The adsorption sampling pipe will carry out aging before collection breath composition;The aging condition is:Ageing gas:Nitrogen, purity For 99.999%;Ageing gas pressure:15-25psi;Aging temperature:280-320℃;Ageing time:20-40min.
9. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 1, it is characterised in that step 2) In, the thermal desorption is carried out in thermal desorption instrument;The condition of the thermal desorption is:Carrier gas:High-purity helium, carrier gas purity >=99.999%;The pre-blowing time:1~4min;One-level is desorbed:Temperature is 220~300 DEG C, and the time is 5~15min, desorption stream Measure as 40~60ml/min;Import is not shunted;Cold hydrazine is in 0~-30 DEG C of enrichments;Two grades of desorptions:Temperature is 250~320 DEG C, when Between be 2~4min;Desorption flow is 15~25ml/min, and outlet manifold, bypass flow is 15~25ml/min.
10. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 1, it is characterised in that step 3) in, the condition of gas chromatography-mass spectrometry is:
The GC conditions are:Chromatographic column:DB-waxlter capillary columns;Thermal desorption and gas-chromatography transmission line temperature:180 ℃;Carrier gas:High-purity helium, carrier gas purity >=99.999%;Flow velocity:0.8-1.2mL/min;Splitless injecting samples;Heating schedule: 40 DEG C of initial temperature, 220 DEG C are risen to 5 DEG C/min speed, keep 5min, and the bulk analysis time is 41min;
The Mass Spectrometry Conditions are:Makings coffret temperature:250℃;Ion source temperature:230℃;Level Four bar temperature:150℃; Solvent delay:0.5min;Ionization mode:EI sources;Ionizing energy:70eV;Scan mode:Full scan (Scan);Quality is swept Retouch scope m/z:29~250amu.
11. the detection method of papermaking-method reconstituted tobaccos material breath composition according to claim 1, it is characterised in that step 3) in, the gas chromatography-mass spectrometry is entered using NIST standard spectrums storehouse to papermaking-method reconstituted tobaccos material breath composition Row library searching is qualitative;The NIST standard spectrums storehouse selects matching degree >=80 to breath composition basis for estimation.
CN201610118551.7A 2016-03-02 2016-03-02 A kind of detection method of papermaking-method reconstituted tobaccos material breath composition Pending CN107153014A (en)

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