CN105865891A - Internal standard substance release and escape product enrichment combination device for thermal analyzer and use method of device - Google Patents
Internal standard substance release and escape product enrichment combination device for thermal analyzer and use method of device Download PDFInfo
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- CN105865891A CN105865891A CN201610344006.XA CN201610344006A CN105865891A CN 105865891 A CN105865891 A CN 105865891A CN 201610344006 A CN201610344006 A CN 201610344006A CN 105865891 A CN105865891 A CN 105865891A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N2001/4038—Concentrating samples electric methods, e.g. electromigration, electrophoresis, ionisation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to an internal standard substance release and escape product enrichment combination device for a thermal analyzer. The combination device comprises a release chamber (10), an enrichment chamber (24) and a sampling needle (21), wherein the release chamber (10) and the enrichment chamber (24) are connected through a transmission pipeline (27), and the sampling needle (21) is inserted into the enrichment chamber (24). A first carrier gas inlet (6) is formed in the upper portion of the release chamber (10), an internal standard solution (2) is contained in the release chamber (10), a second carrier gas inlet (25) is formed in the lower portion of the enrichment chamber (24), the enrichment chamber (24) is provided with an extract liquor attaching device (18), extract liquor drops (17) are suspended on the extract liquor attaching device (18), and a carrier gas outlet (23) is formed in the upper portion of the enrichment chamber (24). A needle tip of the sampling needle (21) is located in the extract liquor drops (17) suspended on the extract liquor attaching device (18), and a point discharge device (15) is further arranged at the bottom of the enrichment chamber (24).
Description
Technical field
The invention belongs to instrument and equipment field, be specifically related to a kind of internal standard substance for thermal analyzer and discharge and ease
Go out the combined apparatus of product enrichment.
Technical background
Thermoanalysis technology is various transformations and the reaction of research material under temperature program(me) control, such as dehydration, knot
Brilliant, melted, evaporation, phase transformation and the thermal decomposition process of various inorganic and organic materials and kinetics problem
Etc., it is a kind of highly important analysis test method.As the one of conventional thermal analytical technology, thermogravimetric/poor
Thermal analysis system be application thermobalance under programed temperature, measurement of species quality, thermal change quality increase,
Mass loss or heat absorption, heat release and a kind of thermoanalysis technology of temperature relation, have instrumentation easy, accurately
Spend high, sensitive quickly and the advantage such as sample milligram ammonia, be widely used in inorganic, organic, chemical industry,
The fields such as metallurgy, medicine, food, Nicotiana tabacum L., the energy and biology.
Liquid-phase micro extraction technique is to propose in the mid-90 in 20th century, and the one developed rapidly is new
The Sample Pretreatment Technique of type.Liquid-phase micro-extraction can provide the sensitivity compared favourably with classical liquid-liquid extraction, very
To more preferably concentration effect；This technology integrates sampling, separation, purification, concentration, sample introduction, and adapts to
Complex dielectrics, trace constituent, the analysis of special nature composition；Simple to operate, quick, it is not necessary to specific apparatus sets
Standby；Extraction mode is many, and available organic solvent kind is many and consumption is the most several to tens microlitres, for optimizing liquid
The condition of phase extraction provides the biggest space.In the present building resource-efficient and environment friendly society
My god, the sample-pretreating method using environmental protection, consumption of organic solvent little and inexpensive has important reality meaning
Justice.The extraction phase of liquid-phase micro-extraction can directly carry out ultraviolet/visible spectrophotometry, fluorescence spectrophotometry,
Atomic absorption spectroscopy determination, it is possible to enter gas chromatograph, high performance liquid chromatograph, efficient capillary
The modern instruments such as electrophresis apparatus, chromatograph-mas spectrometer or capillary electrophoresis-laser-induced fluorescence instrument are analyzed.Liquid phase
Micro-extraction technique is widely used in fields such as environment, food, medicine, active ingredient of Chinese herbs analyses.
Liquid-phase micro-extraction is as a kind of novel sample pretreatment, and collection is sampled, extracted and concentrate in one, has spirit
The advantages such as sensitivity is high, simple to operate, the most cheap, have been developed rapidly and have been carried out at numerous areas
It is widely applied.
Electrostatic generator mainly produces electrostatic, and output is typically single polarity, as positive or negative polarity, defeated
Go out voltage can regulate, be typically used in field of scientific study, electrostatic application such as electrostatic precipitation, electrostatic spraying,
Produce electrostatic field for biological effect research and the place of other electrostatic to be applied.
Summary of the invention
The present invention provide a kind of internal standard substance for thermal analyzer to discharge and the combined apparatus of effusion product enrichment and
Its using method.
It is an object of the invention to provide a kind of effective and feasible combined apparatus for thermal analyzer effusion product analysis,
Internal standard substance release device is utilized to make carrier gas is uniformly carried the internal standard substance component volatilized, in utilizing enriching apparatus to make
Mark thing and effusion product adsorb under the same conditions, extract, are enriched with, it is achieved to reaction effusion product qualitative and
Relative quantification and effusion Behavior law analysis thereof.
It is an object of the invention to the effusion behavior of thermal decomposition product in monitoring reaction course, for complicated thermal chemical reaction
More abundant information is provided, speculates reaction mechanism and target product formation mechanism accordingly, set up thermal chemical reaction
Model, studies the method promoted or suppression target product generates, makes thermal chemical reaction under controllable state
Carry out according to preferable direction.
It is an object of the invention to realize the enrichment continuously to thermal chemical reaction effusion product, sampling, utilize this connection
Coordinate with automatic sampler with device and realize thermal analyzer and gas chromatography-mass spectrum, liquid chromatography-mass spectrography, capillary
The auto injection detection of the analytical tool such as electrophoresis tube.
First aspect present invention provides a kind of internal standard substance for thermal analyzer to discharge and the connection of effusion product enrichment
With device, it includes discharging chamber 10 and the enrichment chamber 24 connected by transfer conduit 27 and being positioned at described richness
Sampling probe 21 in collection top, chamber 24 sample tap 20, described transfer conduit 27 connects on described release chamber 10
Portion and bottom, described enrichment chamber 24；First carrier gas enters described release chamber 10 by the first carrier gas inlet 6 and purges
Described enrichment is entered by described transfer conduit 27 after the liquid level 11 of the inner mark solution 2 in described release chamber 10
Chamber 24, is escaped with the testing sample that carries entered by the second carrier gas inlet 25 of bottom, described enrichment chamber 24
The thermal analyzer carrier gas mixing of product, the mixed carrier gas of formation purges extract attaching in described enrichment chamber 24
From carrier gas outlet 23 effusion after extract drop 17 on device 18；The syringe needle of described sampling probe 21 is positioned at institute
State in the extract drop 17 hung on extract attaching device 18.
In a preferred embodiment of the present invention, dividing plate 9 that can be movable is arranged at top, described release chamber 10, under
Portion equipped with described inner mark solution 2, the liquid level of described inner mark solution 2 by liquid surface height controlling device 4 by the
One sensor 5 be connected the first fluid reservoir 1 and the first of described release chamber 10 having described inner mark solution 2
Fluid discharge pump 3 controls；The liquid level of described dividing plate 9 bottom surface and described inner mark solution 2 determines the district of carrier gas purge
Territory；The gas flow that carrier gas enters described release chamber 10 by the first carrier gas inlet 6 is controlled by gas flow
Device 7 is controlled.
In a preferred embodiment of the present invention, the described sample tap 20 on top, described enrichment chamber 24 is by sealing ring
22 are sealed, and described sample tap 20 bottom connects the conveying pipe 19 of conveying extract, described conveying pipe 19 times
End connects described extract attaching device 18, and described sampling probe 21 penetrates and pass described sealing ring 22 and institute
Enter in the extract drop 17 hung on described extract attaching device 18 after stating conveying pipe 19；Described extraction
The shape taking drop 17 is had described extraction by the second sensor 5a with being connected by droplet profile controller 14
Second fluid reservoir 1a of solution 13 and the second liquid flow pump 3a control of the conveying pipe 19 of described conveying extract
System；Bottom, described enrichment chamber 24 has point discharge device 15, described point discharge device 15 to connect outside
Electrostatic generator 26；It is diagonal upward direction that described transfer conduit 27 enters the Way in described enrichment chamber 24.
In a preferred embodiment of the present invention, described release chamber 10 and described enrichment chamber 24 and described transmission
The temperature of pipeline 27 is controlled by temperature controller 12.
Second aspect present invention provides a kind of internal standard substance for thermal analyzer to discharge and the connection of effusion product enrichment
By the using method of device, it comprises the following steps:
A prepares inner mark solution, joins in the first fluid reservoir 1；
B preparation extraction solution, joins in the second fluid reservoir 1a after filtering；
C puts into testing sample in thermal analyzer, arranges hot analysis condition, and described hot analysis condition includes: just
Beginning temperature, final temperature, heating schedule, experiment atmosphere, carrier gas flux, sample size, reference substance；
D selects carrier gas for release chamber 10, arranges carrier gas flux by gas flow controller 7, regulates dividing plate 9
Highly；
E starts liquid surface height controlling device 4, determines inner mark solution 2 liquid level in release chamber 10；
F start-up temperature controller 12, determines release chamber 10 and described enrichment chamber 24 and described transfer conduit 27
Temperature；
G starts droplet profile controller 14, determines the shape of extract drop 17 drop being enriched with in chamber 24；
H starts electrostatic generator 26 and arranges voltage, determines the discharge effect of point discharge device 15；
I starts thermal analyzer heating schedule, the thermal analysis curve of record detection sample；
J selects multiple time points or temperature spot, sampling probe 21 penetrates sample tap 20 through sealing ring 22
With the conveying pipe 19 of conveying extract, syringe needle is made to be positioned at extract attaching device 18 and hang extraction drop 17
In, extraction extract is also transferred in chromatography column feed materials bottle, is analyzed；
K gathers heat analysis data.
In a preferred embodiment of the present invention, described inner mark solution 2 is prepared by internal standard substance and solvent, described interior
Mark thing has volatility.
In a preferred embodiment of the present invention, the carrier gas entering described release chamber 10 is escaped with carrying testing sample
The thermal analyzer carrier gas going out product is identical or different, enter described release chamber 10 carrier gas maximum flow for
Drop is not splash during purging inner mark solution 2 liquid level.
In a preferred embodiment of the present invention, the carrier gas in described entrance described release chamber 10 treats test sample with carrying
The thermal analyzer carrier gas of product effusion product is noble gas.
In a preferred embodiment of the present invention, described extract be a kind of solvent or the preparation of several solvent and
Become, the analysis detection not disturbing pyrolysis effusion product of the component of described extract.
The invention have the characteristics that:
1, utilize carrier gas purge inner mark solution liquid level, make carrier gas is uniformly carried the internal standard substance component volatilized,
Enrichment chamber makes internal standard substance and pyrolysis effusion product extract under the same conditions, be enriched with, and the pyrolysis effusion to reaction is produced
Thing carries out qualitative and relative quantitative assay research.
2, by adjusting the divider height discharging chamber in internal standard substance release device, reach molten to carrier gas purge internal standard
The accurate control of liquid liquid level effect, liquid surface height controlling device guarantees stablizing of liquid level, thus realizes in carrier gas
Accurately regulation and the stability contorting of internal standard substance content.
3, enrichment chamber utilizes the common effect that Electrostatic Absorption and/or droplet extraction absorb, and flows through the load in enrichment chamber
In gas, internal standard component and pyrolysis effusion product are enriched in drop, utilize sampling probe to extract drop, and device has letter
Just, advantage fast and efficiently, convenient with gas chromatography-mass spectrum, liquid chromatography-mass spectrography, capillary electrophoresis etc.
Analytical tool is combined.
4, droplet profile controller monitoring real-time to droplet size, it is ensured that drop has excellent in shape, sampling probe
Drop can be extracted at any time, it is achieved the continuous sampling to reaction effusion product, with automatic sampler according to experiment needs
Cooperation can realize the auto injection detection of combined analytical instrument.
5, utilize thermal analyzer to obtain the heat analysis data of reaction, utilize this device and combined analytical instrument to obtain
Reaction effusion product qualitative and relative quantitation information and effusion Behavior law, can speculate accordingly reaction mechanism with
Target product formation mechanism, studies the method promoted or suppression target product generates, makes thermal chemical reaction
Carry out according to preferable direction under controllable state.
6, this combined apparatus also can be used for the extraction of volatile component, enrichment in gas, only need to be by gas warp to be measured
It is passed through enrichment chamber by the second carrier gas inlet, the qualitative and relative quantitative assay of volatile component in gas can be carried out.
Accompanying drawing explanation
Fig. 1 is that the internal standard substance for thermal analyzer of the present invention discharges and the combined apparatus figure of effusion product enrichment.
In Fig. 1, reference is: 1 first fluid reservoir；1a the second fluid reservoir；2 inner mark solutions；3—
First liquid flow pump；3a second liquid flow pump；4 liquid surface height controlling devices；5 first sensors；
5a the second sensor；6 first carrier gas inlets；7 gas flow controllers；8 carrier gas flow to；9 every
Plate；10 release chambeies；11 liquid levels；12 temperature controllers；13 extracts；14 droplet profiles control
Device；15 point discharge devices；16 mixed carrier gas flow to；17 extract drops；18 extract attachings
Device；19 conveying pipes；20 sample taps；21 sampling probes；22 sealing rings；23 carrier gas outlets；24
Enrichment chamber；25 second carrier gas inlets；26 electrostatic generators；27 transfer conduit.
Fig. 2 is the thermogravimetric of raw coffee bean powder of the present invention, differential thermal curve figure.
Fig. 3 is the raw coffee bean powder total ions chromatogram pair at different temperatures section effusion product of the present invention
Ratio.
Fig. 4 be the present invention each temperature section total ions chromatogram in the contrast of internal standard substance peak area.
Fig. 5 is the effusion behavior of the reaction effusion product of the present invention.
Detailed description of the invention
For further illustrating technological means and effect of the present invention, below in conjunction with accompanying drawing and preferred embodiment, right
The internal standard substance for thermal analyzer proposed according to the present invention discharges and the combined apparatus application of effusion product enrichment
And embodiment describes in detail as follows, but present disclosure is not limited to this.
Embodiment: thermal analyzer-effusion product enrichment-gas chromatography-mass spectrography postgraduate's coffee bean powder pyrolysis
The effusion behavior of product
The thermobalance sensitivity arranging thermal analyzer is 1 μ g, accurately weighs the raw coffee of 100.00 ± 0.05mg
Coffee bean powder sample is put into the crucible of thermal analyzer and is carried out thermogravimetric test.Temperature programming condition is: with 10 DEG C
The heating rate of/min, is heated to 900 DEG C from 40 DEG C, keeps 10min.Carrier gas is air, flow 200
mL/min。
As in figure 2 it is shown, raw coffee bean powder sample obtain in 40 DEG C to 400 DEG C Temperature Programmed Processes thermogravimetric,
Differential thermal curve figure.Finding out from thermogravimetric curve figure, the thermochemical reaction process that sample occurs does not has obvious platform
Phase, reaction is the not obvious divided stages being carried out continuously.The second step utilizing mass loss bigger is looked for
To the cross point of thermogravimetric curve Yu corresponding tangent line, thermal process reactor is divided into three phases: first stage quality
Loss speed is more slow, and before 215 DEG C, sample weight loss is 9.13%；From 215 DEG C to 343 DEG C
For second stage, sample quality reduces again 42.32%, finds out that there is obvious heat release in this stage from differential thermal curve
Behavior；Being the phase III from 343 DEG C to 400 DEG C, sample weight loss speed slowed down but higher than the first stage,
This stage sample quality reduces 9.73%.
Utilize internal standard substance release and the combined apparatus of effusion product enrichment, at 100 DEG C to 400 DEG C temperature-rise periods
In divide temperature sections sampling enrichment thermal analyzers effusion products according to 20 DEG C of intervals, and pass through gas chromatography-mass spectrum
It is separated, analyzes by instrument, chooses effusion product total ions chromatogram such as Fig. 3 that wherein 5 temperature sections obtain
Shown in.Mass spectrum library searching is utilized to confirm the compound corresponding to each chromatographic peak, retention time 5.0min in figure
The compound at place is the internal standard substance used in combined apparatus, and the ratio of peak of each temperature section internal standard substance is closer to；Remaining
Compound is the effusion product of thermal chemical reaction, it is seen that the component of each temperature section effusion product exists larger difference.
It is illustrated in figure 4 the contrast of internal standard substance peak area in each temperature section total ions chromatogram, abscissa
The initial temperature of temperature value correspondence relevant temperature section, it is therefore seen that the concentration effect that internal standard substance is in drop is by liquid
Drip the impact of the factor such as shape micro-variations and time changing.Internal standard substance and effusion product enrichment in drop
The impact that both are caused by the factors such as journey is simultaneous, droplet profile micro-variations is identical.Internal standard
The use of thing makes the relative amount of different temperatures section effusion product be provided with comparability, eliminates droplet profile microcosmic
The impact that effusion product relative amount is calculated by the factors such as change.Utilize internal standard substance peak area can to revise and calculate
Pyrolysis effusion product, in the relative amount situation of change of different temperatures section, obtains more structurally sound effusion behavior bent
Line.The relative quantitation information of target product can be obtained further in conjunction with heat analysis data.
As it is shown in figure 5, in total ions chromatogram as a example by compound at retention time 9.5min, draw
The effusion behavior in 100 DEG C to 400 DEG C temperature-rise periods of this effusion product, vertical coordinate is compound peaks face
Long-pending through the revised ratio of internal standard substance peak area, the initial temperature of the temperature value correspondence relevant temperature section of abscissa.
This effusion product confirms as pyridine through mass spectrum library searching, finds out that it occurs mainly with from effusion behavior curve
260～280 DEG C and 280～300 DEG C of two temperature sections, with 280～300 DEG C of temperature ranges for mainly escaping district
Between.
Claims (9)
1., for internal standard substance release and the combined apparatus for effusion product enrichment of thermal analyzer, its feature exists
In, it includes discharging chamber (10) and the enrichment chamber (24) connected by transfer conduit (27) and being positioned at institute
Stating the sampling probe (21) in enrichment chamber (24) top sample tap (20), described transfer conduit (27) connects
(10) top, described release chamber and described enrichment chamber (24) bottom；The first carrier gas inlet (6) is passed through in first carrier gas
Enter described release chamber (10) and purge the liquid level (11) of the inner mark solution (2) in described release chamber (10)
Described enrichment chamber (24) is entered afterwards, and by under described enrichment chamber (24) by described transfer conduit (27)
What second carrier gas inlet (25) in portion entered carries the thermal analyzer carrier gas mixing of testing sample effusion product, shape
The mixed carrier gas become is the extract drop on purging extract attaching device (18) in described enrichment chamber (24)
(17) from carrier gas outlet (23) effusion after；The syringe needle of described sampling probe (21) is positioned at described extract attaching
In the upper extract drop (17) hung of device (18).
Combined apparatus the most according to claim 1, it is characterised in that described release chamber (10) top
Have can be movable dividing plate (9), bottom is equipped with described inner mark solution (2), the liquid of described inner mark solution (2)
Face height is had described inner mark solution (2) by first sensor (5) with being connected by liquid surface height controlling device (4)
The first fluid reservoir (1) and described release chamber (10) first liquid flow pump (3) control；Described dividing plate
(9) liquid level of bottom surface and described inner mark solution (2) determines the region of carrier gas purge；First carrier gas passes through first
Carrier gas inlet (6) is entered the gas flow of described release chamber (10) and is controlled by gas flow controller (7)
System.
Combined apparatus the most according to claim 1, it is characterised in that described enrichment chamber (24) top
Described sample tap (20) sealed by sealing ring (22), described sample tap (20) bottom connect conveying extraction
Taking the conveying pipe (19) of liquid, described conveying pipe (19) lower end connects described extract attaching device (18), institute
State sampling probe (21) penetrate and pass described sealing ring (22) and described conveying pipe (19) enter described extraction afterwards
Take in the upper extract drop (17) hung of liquid attaching device (18)；The shape of described extraction drop (17)
Described extraction solution (13) is had by the second sensor (5a) with being connected by droplet profile controller (14)
The second fluid reservoir (1a) and the second liquid flow pump (3a) of conveying pipe (19) of described conveying extract
Control；Point discharge device (15), described point discharge device (15) are arranged at described enrichment chamber (24) bottom
Electrostatic generator (26) outside Lian Jieing；Described transfer conduit (27) enters entering of described enrichment chamber (24)
Mouth direction is diagonal upward direction.
Combined apparatus the most according to claim 1, it is characterised in that described release chamber (10) and institute
The temperature stating enrichment chamber (24) and described transfer conduit (27) is controlled by temperature controller (12).
5. a using method for the combined apparatus being enriched with for internal standard substance release and the effusion product of thermal analyzer,
It is characterized in that, it comprises the following steps:
A prepares inner mark solution, joins in the first fluid reservoir (1)；
B preparation extraction solution, joins in the second fluid reservoir (1a) after filtering；
C puts into testing sample in thermal analyzer, arranges hot analysis condition, and described hot analysis condition includes: just
Beginning temperature, final temperature, heating schedule, experiment atmosphere, carrier gas flux, sample size, reference substance；
D selects the first carrier gas for release chamber (10), arranges carrier gas flux by gas flow controller (7),
Regulation dividing plate (9) is highly；
E starts liquid surface height controlling device (4), determines inner mark solution (2) liquid level in release chamber (10)；
F start-up temperature controller (12), determines release chamber (10) and described enrichment chamber (24) and described biography
The temperature of defeated pipeline (27)；
G starts droplet profile controller (14), determines extract drop (17) liquid in enrichment chamber (24)
The shape dripped；
H starts electrostatic generator (26) and arranges voltage, determines the discharge effect of point discharge device (15)；
I starts thermal analyzer heating schedule, the thermal analysis curve of record detection sample；
J selects multiple time points or temperature spot, sampling probe (21) penetrates sample tap (20) through sealing
Circle (22) and the conveying pipe (19) of conveying extract, make syringe needle be positioned at extract attaching device (18) and hang
Hanging in extraction drop (17), extraction extract is also transferred in chromatography column feed materials bottle, is analyzed；
K gathers heat analysis data.
Using method the most according to claim 5, it is characterised in that described inner mark solution (2) is by interior
Mark thing and solvent preparation, described internal standard substance has volatility.
Using method the most according to claim 5, it is characterised in that enter described release chamber (10)
Carrier gas with carry testing sample effusion product thermal analyzer carrier gas identical or different, enter described release chamber
(10) maximum flow of carrier gas is not for splashing drop when purging inner mark solution (2) liquid level.
Using method the most according to claim 7, it is characterised in that described entrance described release chamber (10)
Carrier gas with carry testing sample effusion product thermal analyzer carrier gas be noble gas.
Using method the most according to claim 5, it is characterised in that described extract is a kind of solvent
Or several solvents are formulated, the analysis detection not disturbing pyrolysis effusion product of the component of described extract.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106248469A (en) * | 2016-10-31 | 2016-12-21 | 钟曼匀 | A kind of continuous micro-extraction device of drop being automatically replenished collection drop and extracting process |
| CN108593487A (en) * | 2018-04-02 | 2018-09-28 | 云南中烟工业有限责任公司 | A kind of gravitational thermal analysis method of the safe temperature window of low temperature cigarette for identification |
| CN109060869A (en) * | 2018-10-15 | 2018-12-21 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction device and method for thermal analyzer evolution component analysis |
| CN113447589A (en) * | 2021-06-30 | 2021-09-28 | 界首市好味来食品有限公司 | Multifunctional food quality detection platform |
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