CN106841374A - The device of inorganic salts ingredients and application in a kind of on-line analysis cigarette ash - Google Patents
The device of inorganic salts ingredients and application in a kind of on-line analysis cigarette ash Download PDFInfo
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Abstract
The invention provides a kind of apparatus and method of inorganic salts ingredients in on-line analysis cigarette ash, on-line analysis system used includes cigarette ash acidizing device, feeder and reaction stream outlet detection means.The on-line analysis are using above-mentioned on-line analysis system, cigarette ash and finite concentration inorganic acid are carried out into acidification reaction, carrier gas is provided by feeder carry acidification reaction product outflow acidizing device, a part for reaction stream outlet is directly entered reaction stream outlet detection means and is analyzed, and remaining is discharged as tail gas.The consumption and concentration of the flow velocity and inorganic acid that change carrier gas can obtain the acidification reaction product of various concentrations, acidification reaction product is directly entered reaction stream outlet detection means without the step such as offline concentration, derivative with carrier gas, simple to operate, analysis is accurate, and measurement accuracy is high.
Description
Technical field
It is exactly specifically profit the present invention relates to a kind of apparatus and method of inorganic salts ingredients in on-line analysis cigarette ash
The inorganic acid of low concentration is mixed with cigarette ash sample with the on-line analysis device, is allowed to acidification reaction, finally
Reaction stream outlet rapidly enters gas-detecting device by gas conduit, so as to realize that the acidifying of on-line analysis cigarette ash is produced
The purpose of thing.
Background technology
It is well known that fire not only causes the heavy losses of property also to cause serious casualties.According to causing
Fire can be divided into natural fire and the fire for causing of artificially setting on fire by the reason for fire.Artificial use of setting on fire more
Some combustion-supporting materials or burning things which may cause a fire disaster, conventional combustion-supporting material have the organic solvents such as diesel oil, gasoline, alcohol and robber cement,
And an important channel of burning things which may cause a fire disaster of setting on fire is the cigarette lighted, therefore effectively distinguish cigarette ashes and other materials
Cigarette ash contributes to public security organ to judge fire type and then infers cause of fire.It is used to analyze cigarette ash in document report
Method be mainly GC or GC-MS, generally combine certain offline sample-pretreating method and complete, if any
Machine solvent extraction is detected to cigarette ash composition.But, sample pre-treatments complex operation, process is cumbersome, consumption
When effort, and Main Analysis pair as if cigarette ash in organic principle, such as multiring aromatic hydrocarbon and polychlorinated biphenyl, but
Cannot analysis and identification inorganic salts so that the accuracy of impact analysis result.
The purpose of this paper is to provide a kind of device and new method for analyzing inorganic salts ingredients in cigarette ash.The method with
Acidification reaction glass tube is the cigarette ash sample in the acidification reaction place of inorganic salts, certain density phosphoric acid and certain mass
Product in this hybrid reaction, then acidification reaction product into reaction stream outlet detection means be Ni63Bear ionogen in source
Ionization analysis is carried out in spectrometer.The method efficiently solves the deficiency of above-mentioned analysis method, realizes quick online
Analysis, it is not necessary to any pre-concentration, derivatization or elution step, for organic and inorganic in cigarette ash in research fire
Composition provides a kind of simple and quick, precise and high efficiency detection means and authentic data.In addition, the device gas circuit
Simply, it is with low cost, it is easy to operation.
The content of the invention
It is an object of the invention to provide a kind of apparatus and method of inorganic salts ingredients in on-line analysis cigarette ash.
The device of inorganic salts ingredients in a kind of on-line analysis cigarette ash, it is characterised in that：Including closed acidification reaction
Pipe, carrier gas ingress pipe, inorganic acid sample cell, feeder and reaction stream outlet detection means；
Closed acidification reaction pipe is provided with for containing the inorganic acid sample cell of inorganic acid fluid and being detachably connected
Inorganic acid fluid entrance and gas vent；
The feeder includes carrier gas source of the gas, and the gas of carrier gas source of the gas is passed through acidification reaction pipe through carrier gas ingress pipe
It is interior；The gas outlet end of carrier gas ingress pipe stretches to the liquid level of acidification reaction bottom of the tube or acidification reaction liquid in pipe
Under；
The gas vent of acidification reaction pipe is connected with the gas sampling mouthful of reaction stream outlet detection means.
The acidification reaction pipe is the double glazing pipe of lower end closed, and unclosed upper end is gas inlet pipe connection
Mouthful, be tightly connected with carrier gas ingress pipe, the side wall of acidification reaction pipe be provided with two respectively with gas vent and inorganic
The connected grass tube of acid solution entrance, the first grass tube is connected with inorganic acid sample cell, and the second grass tube is
Acidification reaction product gas outlet pipe；
The closed hollow tube of one end open that inorganic acid sample cell is made for elastomeric material, the other end；
The inorganic acid that will be contained in it by extruding inorganic acid sample cell during acidifying sends into acidification reaction pipe；
The carrier gas ingress pipe is double glazing pipe, and one end opening, the other end is the hollow sphere end of closing,
The through hole of more than 2 is offered on spheric end, for deriving gas, spheric end close to the bottom of acidification reaction pipe,
To ensure that spheric end is placed in below inorganic acid liquid level, inorganic acid is fully taken out of by carrier gas beneficial to acidification reaction product.
The inorganic acid sample cell and the first grass tube grafting, by inorganic acid sample cell, the elasticity of itself is carried out
Sealing, prevents from being caused when extruding inorganic acid the seepage of inorganic acid, and inorganic acid sample cell can take from the first grass tube
Under, and size is adjustable, is easy to hold the inorganic acid of different volumes, the first grass tube is vertical with acidification reaction pipe
Set.
Carrier gas source of the gas is the dry air after steel cylinder or purification equipped with nitrogen, and carrier gas ingress pipe is provided with quality stream
Amount controller, carrier gas flux is controllable.
The reaction stream outlet detection means is the analytical equipment of direct gas sampling, and predominantly gas sampling is negative
Ion mode on-line mass spectroscopy instrument, is connected by gas conduit with acidification reaction pipe；To the one of acidification reaction outflow gas
Fractional-sample is analyzed, and remaining is discharged as tail gas.
The cavity size of the acidification reaction pipe can be adjusted with the consumption of cigarette ash and inorganic acid, it is ensured that carrier gas ingress pipe
Spheric end be placed in below inorganic acid liquid level.
Operated using any described device in claim 1-6, comprised the following steps：
A. the cigarette ash sample that will accurately weigh is put into acidification reaction pipe, and acidification reaction pipe madial wall is ensured as possible
Face ash-free sample adhesion；
B. carrier gas ingress pipe is put into acidification reaction pipe, is tightly connected, now there is no gas to be passed through；
C. inorganic acid is loaded into inorganic acid sample cell, and inorganic acid sample cell and the sealing of the first grass tube is connected
Connect；
D. gas conduit is connected with reaction stream outlet detection means；
E. inorganic acid is sent into acidification reaction pipe by extruding inorganic acid sample cell, opens quality stream immediately afterwards
Amount controller, is passed through carrier gas, while using reaction stream outlet detection means convection current outlet on-line sampling, obtaining cigarette
The feature spectrogram of inorganic salts ingredients in ash.
The gas conduit is organic polymer material pipe or stainless steel tube；
The inorganic acid is the inorganic acid of mass concentration 1-20%, prevents oxidation of the high concentrated acid to inorganic salts ingredients
With the corrosion of inorganic acid sample cell.
Reaction stream outlet detection means is the negative ion mode on-line mass spectroscopy instrument of gas sampling, using Ni63Ion gun
Reaction stream outlet is ionized, the method can effectively be ionized to the acids of difficult ionization, so that it is special to obtain it
Levy spectrogram.
The wherein acidified reaction of inorganic salts typically results in corresponding inorganic acids, because the ionization energy of inorganic acid is higher,
Therefore Ni63Source is suitable to the ionization of inorganic acid.By typically resulting in acid radical anion after negative ion mass spectrum ionization analysis
Or the cluster ions of acid ion and respective acids neutral molecule.
Brief description of the drawings
Fig. 1 is the schematic device of inorganic salts ingredients in on-line analysis cigarette ash：1- acidification reaction pipes；2- carrier gas is led
Enter pipe；3- spheric ends；4- inorganic acid sample cells；5- feeders；6- carrier gas sources of the gas；7- mass flows are controlled
Device；8- reaction stream outlet detection means；9- inorganic acids；The grass tubes of 10- first；The grass tubes of 11- second；
12- gas conduits.
Fig. 2 is six kinds of feature spectrograms of different brands cigarette ashes；
Fig. 3 is the cigarette ash feature spectrogram that two kinds of scenes of fire are extracted.
Specific embodiment
First, Fig. 1 is a kind of device of inorganic salts ingredients in on-line analysis cigarette ash, it is characterised in that：Including close
Acidification reaction pipe 1, carrier gas ingress pipe 2, inorganic acid sample cell 4, feeder 5 and the reaction stream outlet for closing
Detection means 8；
Closed acidification reaction pipe 1 is provided with for containing the inorganic acid sample cell 4 of inorganic acid fluid and detachably connecting
The inorganic acid fluid entrance and gas vent for connecing；
The feeder 5 includes carrier gas source of the gas 6, and the gas of carrier gas source of the gas 6 is passed through acid through carrier gas ingress pipe 2
Change in reaction tube 1；The gas outlet end of carrier gas ingress pipe 2 stretches to the bottom of acidification reaction pipe 1 or acidification reaction
In pipe 1 under the liquid level of liquid；
The gas vent of acidification reaction pipe 1 is connected with the gas sampling mouthful of reaction stream outlet detection means 8.
The acidification reaction pipe 1 is the double glazing pipe of lower end closed, and unclosed upper end is gas inlet pipe company
Interface, is tightly connected with carrier gas ingress pipe 2, the side wall of acidification reaction pipe 1 be provided with two respectively with gas vent
The grass tube being connected with inorganic acid fluid entrance, the first grass tube 10 is connected with inorganic acid sample cell 4, the
Two grass tubes 11 are acidification reaction product gas outlet pipe；
The closed hollow tube of one end open that inorganic acid sample cell 4 is made for elastomeric material, the other end；
The inorganic acid 9 that will be contained in it by extruding inorganic acid sample cell 4 during acidifying sends into acidification reaction pipe 1；
The carrier gas ingress pipe 2 is double glazing pipe, and one end opening, the other end is the hollow sphere end of closing
3, the through hole of more than 2 is offered on spheric end 3, for deriving gas, spheric end 3 is close to acidification reaction
The bottom of pipe 1, to ensure that spheric end 3 is placed in below the liquid level of inorganic acid 9, beneficial to acidification reaction product by carrier gas
Fully take inorganic acid 9 out of.
4 and first grass tube of inorganic acid sample cell 10 grafting, by inorganic acid sample cell 4 itself
Elasticity is sealed, and prevents from causing the seepage of inorganic acid 9 when extruding inorganic acid 9, and inorganic acid sample cell 4 can be from
First grass tube 10 is removed, and size is adjustable, is easy to hold the inorganic acid 9 of different volumes, the first glass
Conduit 10 is vertically arranged with acidification reaction pipe 1.
Carrier gas source of the gas 6 is the dry air after steel cylinder or purification equipped with nitrogen, and carrier gas ingress pipe 2 is provided with matter
Amount flow controller 7, carrier gas flux is controllable.
The reaction stream outlet detection means 5 is the analytical equipment of direct gas sampling, predominantly gas sampling
Negative ion mode on-line mass spectroscopy instrument, is connected by gas conduit 12 with acidification reaction pipe 1；To acidification reaction stream
A part of sampling analysis of outlet, remaining is discharged as tail gas.
The cavity size of the acidification reaction pipe 1 can be adjusted with the consumption of cigarette ash and inorganic acid 9, it is ensured that carrier gas is led
The spheric end 3 for entering pipe 2 is placed in below the liquid level of inorganic acid 9.
Operated using any described device in claim 1-6, comprised the following steps：
A. the cigarette ash sample that will accurately weigh is put into acidification reaction pipe 1, is ensured in acidification reaction pipe 1 as possible
Side wall ash-free sample adhesion；
B. carrier gas ingress pipe 2 is put into acidification reaction pipe 1, is tightly connected, now there is no gas to be passed through；
C. inorganic acid 9 is loaded into inorganic acid sample cell 4, and by inorganic acid sample cell (4 and first grass tube
10 are tightly connected；
D. gas conduit 12 is connected with reaction stream outlet detection means 5；
E. inorganic acid 9 is sent into acidification reaction pipe 1 by extruding inorganic acid sample cell 4, is opened immediately afterwards
Mass flow controller 7, is passed through carrier gas, while being adopted online using the convection current outlet of reaction stream outlet detection means 2
Sample, obtains the feature spectrogram of inorganic salts ingredients in cigarette ash.
The gas conduit 12 is organic polymer material pipe or stainless steel tube；
The inorganic acid 9 is the inorganic acid of mass concentration 1-20%, prevents high concentrated acid to the oxygen of inorganic salts ingredients
Change the corrosion with inorganic acid sample cell 4.
Reaction stream outlet detection means 2 is the negative ion mode on-line mass spectroscopy instrument of gas sampling, using Ni63Ion
Source is ionized to reaction stream outlet, and the method can effectively be ionized to the acids of difficult ionization, so as to obtain it
Feature spectrogram.
Wherein, acidification reaction pipe uses internal diameter about 20mm, the glass tube of length about 12cm, carrier gas ingress pipe
Using internal diameter about 4mm, external diameter about 6mm, the glass tube being tightly connected with grournd glass with acidification reaction pipe.
In addition, gas conduit uses the polyfluortetraethylene pipe of external diameter 4mm, reaction stream outlet detection means uses Ni63
The time of-flight mass spectrometer of source ionization, the mass spectrograph is designed using orthogonal acceleration, is detected with MCP detectors,
A part for reaction stream outlet is analyzed by polyfluortetraethylene pipe into mass spectrograph, and remaining is discharged as waste gas.
Ionized region total gas pressure maintains 75Pa or so in experiment.
Embodiment 1
For the examination of the apparatus and method performance of inorganic salts ingredients in a kind of on-line analysis cigarette ash of the present invention,
Experiment with six kinds of different brands cigarette ashes be object, using their acidifying of the on-line analysis device on-line analysis
Product, to determine contained inorganic salts ingredients.It is set into the flow of high-purity dry air of acidification reaction pipe
It is 1L/min, inorganic acid used is 5% H3PO4, cigarette ash quality is 0.1g, adds H3PO4About 3ml.
In view of the difficult ionization property of inorganic acid, the ionization mode of ionization source uses Ni in experiment63Ion gun, ionized region gas
Pressure maintains 75Pa or so.3ml H are added in the case of ash-free before this3PO4Enter line blank test, sample
Time is 10min.Afterwards, 0.1g cigarette ashes and 3ml H are added in a clean acidification reaction pipe3PO4,
It is quick to be passed through carrier gas and using mass spectrograph carry out sampling analysis immediately.Fig. 2 is six kinds of different brands cigarette ashes
Feature spectrogram.Mass number and relative intensity deduction according to quasi-molecular ions, carbonate is contained in six kinds of cigarette ashs
(HCO2 -, m/z=45；), villaumite (35Cl-With37Cl-, m/z=35 and 37), nitric acid and nitrite (NO3 -,
M/z=62；NO2 -, m/z=46；HNO2.OCN-, m/z=89) and cyanate (OCN-, m/z=42；H2O.OCN-,
M/z=60；HOCN.OCN-, m/z=85；HNO2.OCN-, m/z=89), but their feature spectrogram
Signal intensity difference is very big.Above-mentioned quasi-molecular ions is the feature spectral peak of inorganic salts ingredients in cigarette ashes, for area
Divide cigarette ashes and other cigarette ash compositions.
Embodiment 2
For the examination of the apparatus and method performance of inorganic salts ingredients in a kind of on-line analysis cigarette ash of the present invention,
It is object to test the cigarette ash extracted with two kinds of scenes of fire, using their acid of the on-line analysis device on-line analysis
Change product, to determine contained inorganic salts ingredients.It is set into the stream of high-purity dry air of acidification reaction pipe
It is 1L/min to measure, and inorganic acid used is 5% H3PO4, cigarette ash quality is 0.1g, adds H3PO4About 3ml.
In view of the difficult ionization property of inorganic acid, the ionization mode of ionization source uses Ni in experiment63Ion gun, ionized region gas
Pressure maintains 75Pa or so.3ml H are added in the case of ash-free before this3PO4Enter line blank test, sample
Time is 10min.Afterwards, 0.1g cigarette ashes and 3ml H are added in a clean acidification reaction pipe3PO4,
It is quick to be passed through carrier gas and using mass spectrograph carry out sampling analysis immediately.Fig. 3 is the cigarette ash that two kinds of scenes of fire are extracted
Feature spectrogram.It can be found that lacking quasi-molecular ions NO in the spectrogram of scene ash 12 -, m/z=46 and HNO2.OCN-,
M/z=89, illustrates do not have nitrite in live ash 1, and the spectrogram of scene ash 2 lacks quasi-molecular ions HCO2 -,
M/z=45, HOCN.OCN-, m/z=85, NO2 -, m/z=46 and HNO2.OCN-, m/z=89, explanation
Do not exist carbonate and nitrite in live ash 2.Therefore, it can tentatively judge that both live ashes do not have
Cigarette ashes.
Claims (9)
1. in a kind of on-line analysis cigarette ash inorganic salts ingredients device, it is characterised in that：Including closed acidifying
Reaction tube (1), carrier gas ingress pipe (2), inorganic acid sample cell (4), feeder (5) and reaction stream
Outlet detection means (8)；
Closed acidification reaction pipe (1) be provided with for contain the inorganic acid sample cell (4) of inorganic acid fluid with can
Dismantle the inorganic acid fluid entrance and gas vent of connection；
The feeder (5) includes carrier gas source of the gas (6), and the gas of carrier gas source of the gas (6) is imported through carrier gas
Pipe (2) is passed through in acidification reaction pipe (1)；It is anti-that the gas outlet end of carrier gas ingress pipe (2) stretches to acidifying
Should manage under the liquid level of (1) bottom or acidification reaction pipe (1) interior liquid；
The gas vent of acidification reaction pipe (1) is connected with the gas sampling mouthful of reaction stream outlet detection means (8).
2. device according to claim 1, it is characterised in that：
The acidification reaction pipe (1) is the double glazing pipe of lower end closed, and unclosed upper end is gas access
Tube connection ports, are tightly connected with carrier gas ingress pipe (2), and the side wall of acidification reaction pipe (1) is provided with two difference
The grass tube being connected with gas vent and inorganic acid fluid entrance, the first grass tube (10) and inorganic acid sample
Pipe (4) is connected, and the second grass tube (11) is acidification reaction product gas outlet pipe；
The closed hollow tube of one end open that inorganic acid sample cell (4) is made for elastomeric material, the other end；
The inorganic acid (9) that will be contained in it by extruding inorganic acid sample cell (4) during acidifying sends into acidification reaction
Pipe (1)；
The carrier gas ingress pipe (2) is double glazing pipe, and one end opening, the other end is the hollow ball of closing
Shape end (3), offers the through hole of more than 2 on spheric end (3), for deriving gas, spheric end (3)
Close to the bottom of acidification reaction pipe (1), to ensure that spheric end (3) is placed in below inorganic acid (9) liquid level,
Fully taken out of inorganic acid (9) by carrier gas beneficial to acidification reaction product.
3. device according to claim 2, it is characterised in that：
The inorganic acid sample cell (4) and the first grass tube (10) grafting, by inorganic acid sample cell (4)
The elasticity of itself is sealed, and prevents from being caused when extruding inorganic acid (9) seepage of inorganic acid (9), inorganic acid
Sample cell (4) can be removed from the first grass tube (10), and size is adjustable, is easy to hold different volumes
Inorganic acid (9), the first grass tube (10) is vertically arranged with acidification reaction pipe (1).
4. device according to claim 1, it is characterised in that：
Carrier gas source of the gas (6) is the dry air after steel cylinder or purification equipped with nitrogen, on carrier gas ingress pipe (2)
Mass flow controller (7) is provided with, carrier gas flux is controllable.
5. device according to claim 1, it is characterised in that：
The reaction stream outlet detection means (5) is the analytical equipment of direct gas sampling, and predominantly gas enters
The negative ion mode on-line mass spectroscopy instrument of sample, is connected by gas conduit (12) with acidification reaction pipe (1)；It is right
Acidification reaction flows out a part of sampling analysis of gas, and remaining is discharged as tail gas.
6. device according to claim 1, it is characterised in that：
The cavity size of the acidification reaction pipe (1) can be adjusted with the consumption of cigarette ash and inorganic acid (9), it is ensured that
The spheric end (3) of carrier gas ingress pipe (2) is placed in below inorganic acid (9) liquid level.
7. a kind of any described devices of claim 1-6 inorganic salts ingredients in on-line analysis cigarette ash analyze process
Application, it is characterised in that：
Operated using any described device in claim 1-6, comprised the following steps：
A. the cigarette ash sample that will accurately weigh is put into acidification reaction pipe (1), and acidification reaction pipe is ensured as possible
(1) interior sidewall surface ash-free sample adhesion；
B. carrier gas ingress pipe (2) is put into acidification reaction pipe (1), is tightly connected, now there is no gas
It is passed through；
C. inorganic acid (9) is loaded into inorganic acid sample cell (4), and by inorganic acid sample cell (4) and the
One grass tube (10) is tightly connected；
D. gas conduit (12) is connected with reaction stream outlet detection means (5)；
E. inorganic acid (9) is sent into acidification reaction pipe (1) by extruding inorganic acid sample cell (4), it
Open mass flow controller (7) immediately afterwards, carrier gas is passed through, while using reaction stream outlet detection means (2)
Convection current outlet on-line sampling, obtains the feature spectrogram of inorganic salts ingredients in cigarette ash.
8. application according to claim 7, it is characterised in that：
The gas conduit (12) is organic polymer material pipe or stainless steel tube；
The inorganic acid (9) is the inorganic acid of mass concentration 1-20%, prevents high concentrated acid to inorganic salts ingredients
Oxidation and inorganic acid sample cell (4) corrosion.
9. application according to claim 7, it is characterised in that：
Reaction stream outlet detection means (2) is the negative ion mode on-line mass spectroscopy instrument of gas sampling, using Ni63
Ion gun is ionized to reaction stream outlet, and the method can effectively be ionized to the acids of difficult ionization, so as to obtain
Obtain its feature spectrogram.
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| CN109900835A (en) * | 2017-12-11 | 2019-06-18 | 中国科学院大连化学物理研究所 | The device of inorganic constituents and application in a kind of highly sensitive on-line checking cigarette ash |
| CN110297067A (en) * | 2018-11-12 | 2019-10-01 | 杭州超钜科技有限公司 | Integrated water mercury pretreatment unit and its preprocess method |
| CN110687248A (en) * | 2019-01-30 | 2020-01-14 | 杭州超钜科技有限公司 | System and method for rapidly detecting trace mercury in liquid |
| CN111122688A (en) * | 2019-11-25 | 2020-05-08 | 应急管理部沈阳消防研究所 | Fire material evidence identification method for cigarette combustion ash |
| 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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