CN109991345A - Equipment for being detected to sample gas and the method that sample gas is detected by flame ionization detector - Google Patents
Equipment for being detected to sample gas and the method that sample gas is detected by flame ionization detector Download PDFInfo
- Publication number
- CN109991345A CN109991345A CN201910376464.5A CN201910376464A CN109991345A CN 109991345 A CN109991345 A CN 109991345A CN 201910376464 A CN201910376464 A CN 201910376464A CN 109991345 A CN109991345 A CN 109991345A
- Authority
- CN
- China
- Prior art keywords
- gas
- compensation
- sample
- combustion
- flame ionization
- 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
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention relates to a kind of equipment for being detected to sample gas, equipment includes flame ionization detector, flame ionization detector includes sample gas import, combustion gas inlet and combustion-supporting gas import, in flame ionization detector, the sample gas for flowing into flame ionization detector ionizes under the action of by burning gases and the flame of combustion-supporting gas generation, thus the signal for carrying out chemical analysis to sample gas is generated, equipment further includes compensation gas feeding mechanism, to provide compensation gas to flame ionization detector, to eliminate or mitigate the interference as caused by oxygen existing for itself in sample gas, compensation gas is oxygen-containing gas.The present invention also provides a kind of methods detected by flame ionization detector to sample gas.By the device and method, the oxygen in oxygenous sample gas can be solved to the interference problem of testing result.
Description
Technical field
The present invention relates to a kind of equipment for being detected to sample gas, which includes flame ionization detector.This
Outside, the invention further relates to a kind of methods detected by flame ionization detector to sample gas, wherein sample gas to be detected
In usually contain oxygen gas component.
Background technique
Gas chromatographic analysis is important one of modern age analysis means.On the one hand, it has separation efficiency height, analysis speed
Fastly, quantitative result is accurate, is easy to the features such as automating.On the other hand, gas-matter is carried out when itself and mass spectrograph, computer etc. combine
When combination analysis, qualitative and quantitative analysis can be carried out to complicated multicomponent mixture.Therefore, gas chromatographicanalyzer device is increasingly
The every field such as petrochemical industry, medicine, biochemistry, environmental science are widely used in, industrial and agricultural production, scientific research, teaching etc. are become
Department indispensable important separation and analysis tool.
Gas chromatographicanalyzer device, such as online volatile organic matter analysis generally, based on gas chromatographic analysis principle
Instrument includes a kind of detecting instrument, such as (hydrogen) flame ionization detector (FID).This flame ionization ditector (FID)
The ionic current generated by passive electrode detection when having imported the sample airs such as exhaust to hydrogen flame, and according to by the receipts
The ionic current that collector detects measures the concentration contained by sample air as the hydrocarbon of measurement object substance.Hydrogen flame from
Sonization detector is arranged on the exhaust flow path that sample air (also referred to as sample gas) is flowed through.
When flame ionization detector (FID) be applied to lab analysis when, commonly using inert gas, for example nitrogen or
Helium is as the compensation gas for promoting sample gas, so that sample gas is usually to be present in nitrogen or other inert gases.Standard Gases
Body is typically also to be diluted in nitrogen or other inert gases, so simultaneously not to be noted there is the oxygen content pair in sample gas
The influence of FID testing result.
In addition, being also often used compensation gas or auxiliary gas in the application of flame ionization detector (FID), mainly
It is after first mixing inert gas, such as nitrogen or helium with burning gases (for example, hydrogen), then mixed gas is made to enter fire
It burns in flame ionization detector.Enter the speed of detector, its purpose is to improve sample gas can reach appropriate
Sensitivity, and can increase the turnover rate of sample gas, achieve the purpose that modification tests and analyzes result.
However, by gas-chromatography with hydrogen flame ionization detector application in an atmosphere or the field of uncertain oxygen concentration
When carrying out the detection of sample gas in institute, the variation of sensitivity can occur because the oxygen content in sample gas is different.In addition, flame combustion pair
The degree of functional group's ionization is different, will also result in sensitivity difference, leads to the deviation of final detection result.For example, in reality
Test it has been found that because sample gas in oxygen exist, cause measured deviation that may be up to the full scale of 3%-20%, it is apparent that
Such deviation is not received in this field.
Therefore, exist always to more accurate testing result in the field of gas-chromatography hydrogen flame ionization detector
Demand will especially solve the interference problem when in sample gas including uncertain oxygen content to testing result.
Summary of the invention
The present invention provides a kind of equipment for being detected to sample gas, and the equipment includes flame ionization detector,
The flame ionization detector includes the import of sample gas, combustion gas inlet and combustion-supporting gas import, in the flame ion
In detector, the sample gas of the flame ionization detector is flowed into the effect by burning gases and the flame of combustion-supporting gas generation
It is lower to ionize, thus generate the signal for carrying out chemical analysis to the sample gas, which is characterized in that the equipment further includes
Compensation gas feeding mechanism, to provide compensation gas to the flame ionization detector, to eliminate or mitigate by the sample gas
In interference caused by existing oxygen itself, wherein the compensation gas is oxygen-containing gas.
In addition, the present invention also provides a kind of methods detected by flame ionization detector to sample gas, described
In flame ionization detector, the sample gas of the flame ionization detector is flowed by burning gases and combustion-supporting gas generation
It is ionized under the action of flame, thus generates the signal for carrying out chemical analysis to the sample gas, which is characterized in that institute
It states flame ionization detector and compensation gas is provided, done as caused by the oxygen for including in the sample gas with eliminating or mitigating
It disturbs, wherein the compensation gas is oxygen-containing gas.
By the device and method, the oxygen in oxygenous sample gas can solve to the interference problem of testing result, i.e.,
The interference of oxygen can be eliminated, mitigated by the compensation gas in oxygen-containing gas form provided to flame ionization detector.
Advantageously, compensation gas is air.Air is the choosing of more satisfactory oxygen-containing gas as the gas source of acquirement is facilitated
?.
Advantageously, which includes: sample air pipe, and sample air pipe is connected to the sample gas import；Combustion gas line, combustion
It burns gas piping and is connected to combustion gas inlet；Wherein, compensation gas feeding mechanism includes: compensation gas feeding pipe；Gas
Mixing arrangement, compensation gas feeding pipe by gas mixer and at least one in sample air pipe and combustion gas line
Person is in fluid communication, so that the compensation gas can mix in advance before entering the flame ionization detector with corresponding gas
It closes.
By the structure of this mixed compensation gas and other gases, sensitivity can be more preferably improved.
Preferably, compensation gas feeding pipe can only connect with one of sample air pipe and combustion gas line fluid
It is logical.When compensation gas and sample gas are pre-mixed, can greatly improve into the sample gas of flame ionization detector
Flow.
Turn it is particularly preferred that compensation gas feeding pipe is implemented as using a part in combustion-supporting gas as compensation gas
Move on to the transfer conduit in burning gases.The compensation gas for being directly derived from combustion-supporting gas makes entire pipeline arrangement more flexible, empty
Between more save and cost be also minimized.
In addition, compensation gas feeding mechanism includes being constructed to be permeable to adjust the compensation gas supplied to flame ionization detector
Flow gas flow adjusting means, in order to change the flow of compensation gas in real time or as needed.
In one embodiment, when the flow of the sample gas is 30cc/ minutes, the burning gases (for example, hydrogen)
When flow is 30cc/ minutes, the flow of the compensation gas is adjusted to 5-65cc/ minutes by the compensation gas feeding mechanism.
When the flow of compensation gas in the above range when, the effect that may be implemented more meets the desired requirement of experiment.
In particular, when the flow of the combustion-supporting gas (for example, air) is 250-300cc/ minutes, the compensation gas
Feeding mechanism by the flow of the compensation gas it is adjustable be 5cc/ minutes, 45cc/ minutes or 65cc/ minutes so that by
Deviation caused by oxygen in sample gas can be modified with calculation, to reach more accurate analysis result.
Detailed description of the invention
Fig. 1 shows the equipment according to an embodiment of the invention for being detected to sample gas, and there is shown with will send
Enter sample gas, burning gases, combustion-supporting gas and the compensation gas being pre-mixed with burning gases of flame ionization detector；
Fig. 2 shows the equipment for being detected to sample gas according to another embodiment of the invention, and there is shown with will
It is sent into sample gas, burning gases, combustion-supporting gas and the compensation gas being pre-mixed with sample gas of flame ionization detector；
Fig. 3 shows the equipment for being detected to sample gas according to still another embodiment of the invention, and there is shown with will
It is sent into sample gas, burning gases, combustion-supporting gas and the compensation gas being pre-mixed with sample gas of flame ionization detector；
Fig. 4 A-4C is exemplarily illustrated the detection that can get the fiducial value at oxygen peak under the various pressure of various compensation gas
Data drawing list；And
Fig. 5 is exemplarily illustrated under the different flow of compensation gas oxygen to the comparison diagram of sample gas annoyance level.
It should be noted that the attached drawing of reference is not all drawn to scale, but can expand to illustrate each aspect of the present invention, and
This respect, attached drawing are not necessarily to be construed as restrictive.
Specific embodiment
The invention mainly relates to a kind of equipment for being detected to sample gas.The equipment includes flame ion detection
Device, with the chemical component in detection and analysis sample gas, such as volatile organic matter.Equipment of the invention is especially suitable for including one
Determine the sample gas of amount of oxygen, such as the sample gas directly acquired from the exhaust of air or other aerobic environments.
As already described, in the oxygen containing situation of sample gas, the change of sensitivity can occur because the oxygen content in sample gas is different
The degree that change and flame combustion ionize functional group is different, will also result in sensitivity difference, leads to final detection result
Deviation.
The flame ionization detector 100 being related to herein is, for example, flame ionization ditector.The fire of this type
Flame ionization detector uses hydrogen as burning gases.Preferably, flame ion inspection is also fed into using air as combustion-supporting gas
It surveys in device.But oxygen containing other gases can also be used as combustion-supporting gas and be supplied to flame ionization detector.According to the present invention, exist
Preferred air-fuel ratio when burning in combustion chamber is 10:1, but may be other values.
Additionally, it is often necessary to carry out (usually in advance) diluted sample gas by carrier gas (being mostly nitrogen or helium), so that sample
Gas can be brought into flame ionization detector (for example, with flow of 30 ml/mins).Not by carrier gas encirclement/diluted sample gas
The electric signal (for example, gentle interminable signal curve) that can not be analyzed may be generated.Usually use nitrogen or helium as
The reason of carrier gas is that these gases are relatively stable, will not influence the combustion process conducted in flame ionization detector.
In general, sample gas (for example, 1-5 ml/min) first passes through chromatographic column before entering flame ionization detector 100
Progress ingredient (physical/chemically) separation, in order to constituent analysis.When by chromatographic column, sample gas (is carried) by carrier gas
Flow velocity it is relatively slow (for example, 30 ml/mins), to facilitate carry out lock out operation.And after leaving chromatographic column, it is expected that sample
Flow velocity of the gas in flame ionization detector improves.
Therefore, in the present invention, the speed into flame ionization detector is improved using compensation gas or auxiliary gas
Degree, and thus to obtain sensitivity appropriate, achieve the purpose that modification analysis result (that is, reducing or eliminating the oxygen pair in sample gas
As a result influence).Therefore, to be clearly function different two for " compensation gas/auxiliary gas " and " carrier gas " under meaning of the present invention
Kind gas.In the prior art, even with compensation gas/auxiliary gas, the indifferent gas such as nitrogen or helium are generally also selected
Body.
As an example, during being detected by flame ionization detector 100, by (chromatography post separation
Sample gas (that is, under test gas), carrier gas (for example, nitrogen or helium), burning gases (hydrogen), combustion-supporting gas are (for example, empty afterwards)
Gas) combustion chamber of flame ionization ditector is passed through via respective import (or having mixed before entering), light hydrogen
Gas forms hydrogen flame.It is fixed on flame ionization ditector in general, passive electrode and polarizing electrode pass through insulator respectively,
Passive electrode is connect to the anode of DC power supply, and polarizing electrode is connect to the cathode of DC power supply, in passive electrode and polarization electricity
It produces between pole at DC voltage, to form ionizing electric field.The inside of combustion chamber generates high temperature, sample gas and load because of combustion of hydrogen
Chemi-ionization occurs through high temperature for gas, and ionization generates negative ions in ionizing electric field to respectively opposite electrode movement, formed
Ion stream be collected electrode receive, output, become electric signal through impedance conversion, amplifier amplification, record as representing
The analysis of spectra of material composition and content, and the gas after burning is discharged from exhaust outlet.
For this purpose, flame ionization detector 100 according to the present invention may include sample gas import 10,20 and of combustion gas inlet
The import independent of each other such as combustion-supporting gas import 30 and for after burning gas discharge flame ionization detector 100 extremely
A few exhaust outlet.
In order to solve the problems, such as that testing result has significant deviation in the oxygen containing situation of sample gas, inventor is attempted to GC gas
Mutually the isolation technics of chromatography is by the volatile organic compounds (VOC) and oxygen separation in sample gas, then again by the oxygen after separation
The signal of the signal that gas senses on flame ionization ditector and unsegregated volatile organic compounds (VOC) is direct
Subtract each other.
However, inventors realized that, relationship between the two signal is not linear, therefore this side directly subtracted each other
Method cannot be removed effectively this deviation.This is because the oxygen contained in sample gas is also assisted in the combustion process in combustion chamber,
And affect the numerical value of the aforementioned air-fuel ratio limited by combustion-supporting gas and burning gases.
Therefore, according to the present invention, inventor creatively uses oxygen-containing gas as compensation gas, rather than such as existing
Using inert gases such as nitrogen or helium as known in technology.For example, compensation gas can (oxygen contains for air
Amount is usually 21% or so) or any gas comprising oxygen.
As shown in exemplary in Fig. 4 A-4C, when nitrogen and air is respectively adopted as compensation gas, oxygen peak-to-peak signal exists
Under each flow condition (0.00cc/ minutes, 5.66cc/ minutes and 60.00cc/ minutes) numerical value (be embodied in voltage value,
Volt).
Specifically, Fig. 4 A-4C includes two curves, darker curve (the lower song in upper curve or Fig. 4 B in Fig. 4 A, 4C
Line) it is the experimental data carried out in the case where being passed through pure nitrogen gas as sample gas.It can be seen that in the sample gas of nitrogen balance,
Because being changed significantly without oxygen without the changes in flow rate with compensation gas.Lighter curve is (under in Fig. 4 A, 4C
Upper curve in curve or Fig. 4 B) it is the experimental data carried out in the case where being passed through pure air as sample gas, due in sample gas
There are oxygen thus as the changes in flow rate of compensation gas can have significant change.
More specifically, the box 1 marked in Fig. 4 A-4C indicates in chromatography separating method, in above-mentioned each analysis condition
In, such as will appear between 40-50 seconds the signal peak (can be described as " oxygen peak ") of oxygen.The signal peak of this oxygen can be with increasing
Add the flow of compensation gas and change, such as the variation tendency from the left side of Fig. 4 to right side is first to be stepped up, be reduced to again
Almost without.
Meanwhile the box 2 marked in Fig. 4 A-4C then indicates: the signal peak of measurement as the flow of compensation gas not
Influence peak area together.For example, the peak area at the signal peak is larger when the flow of compensation gas is 5.66cc/ minutes.
In addition, the box 3 that marks in Fig. 4 A-4C indicates: voltage baseline also can with the difference of the flow of compensation gas and
Cause the variation of voltage levels.
Here, compensation gas is mainly used for eliminating or at least mitigating in sample gas caused by existing oxygen itself to detection
As a result interference." eliminating or mitigate " under meaning of the invention can be for example including to itself existing oxygen content in sample gas
Quantify/modified process.
For this purpose, equipment according to the present invention includes compensation gas feeding mechanism, to provide to flame ionization detector 100
Compensation gas (i.e., makes oxygen-containing gas flow into the inside of the flame ionization detector 100 as compensation gas).
It in some embodiments, can be directly by the compensation gas feeding mechanism (for example, its pipeline) by compensation gas
It is sent into flame ionization detector 100 (for example, via an independent compensation gas import).
But in further embodiments, compensation gas is not sent directly into flame ionization detector 100, but will mend
Repay gas be sent into before flame ionization detector 100 by its gas with other flame ionization detectors 100 to be sent into
Row is pre-mixed.For this purpose, compensation gas feeding mechanism of the invention may include various forms of gas mixers.
For example, as shown in fig. 1, burning gases (hydrogen), combustion-supporting gas and sample gas respectively along combustion gas line 22,
Combustion-supporting gas pipeline 32, sample air pipe 12 and via respective import (i.e., combustion gas inlet 20, combustion-supporting gas import 30, sample
Gas import 10) it is admitted in flame ionization detector 100.
Compensation gas feeding mechanism according to the present invention includes compensation gas feeding pipe 50, to convey compensation gas.This
Outside, compensation gas feeding mechanism further includes gas mixer, and the gas mixer is for making compensation gas enter flame
Before ionization detector 100 first by the burning gases (hydrogen) of compensation gas and flame ionization detector 100 to be sent into and
At least one of sample gas is mixed.Therefore, compensation gas feeding pipe 50 by the gas mixer and with sample gas
At least one of pipeline 12 and combustion gas line 22 are in fluid communication.
In some embodiments, compensation gas feeding pipe 50 can each lead into sample air pipe 12 and combustion gas line
22.Compensation gas feeding pipe 50 may include the Liang Ge branch separated from same pipeline, the two branches each lead into sample gas
Pipeline 12 and combustion gas line 22.But compensation gas feeding pipe 50 can also be constructed for two pipes independent of each other in itself
Road, to each lead into sample air pipe 12 and combustion gas line 22.
In further embodiments, compensation gas feeding pipe 50 is only and in sample air pipe 12 and combustion gas line 22
One is in fluid communication, and is attached to sample air pipe 12 (as shown in Figure 2) or combustion gas line 22 (such as institute in Fig. 1 and Fig. 3
Show).
In general, compensation gas feeding pipe 50 may include opposite first end and second end.At first end, gas is compensated
Body feeding pipe 50 and sample air pipe 12 or with 22 flow communication of combustion gas line, and at second end, compensation gas supply
Pipeline 50 is connected with compensation gas source (can integrate or be not integrated into the equipment for being detected to sample gas).But it can be with
It is understood that in the embodiment that compensation gas feeding pipe 50 each leads into sample air pipe 12 and combustion gas line 22, compensation
The first end of gas feed line 50 may include each leading into two first ends of sample air pipe 12 and combustion gas line 22,
And second end can be merged into an end being connected with compensation gas source or be also possible to separate two second ends.
As shown in Figure 2, burning gases (such as hydrogen), combustion-supporting gas (such as air) and sample gas are respectively via respective
Import is admitted in flame ionization detector 100.The gas mixer of compensation gas feeding mechanism first by compensation gas with
The sample gas of flame ionization detector 100 to be sent into directly first is mixed, then through mixed sample gas via sample gas import 10
It is admitted to flame ionization detector 100.For this purpose, the gas mixer may include being sent into from compensation gas source by compensation gas
The feeding pipe of sample air pipe.
In a preferred embodiment, compensation gas is not from independent compensation gas source, but by equipment or
Existing gas source in system.For example, as shown in fig. 1, a part in combustion-supporting gas is supplied directly to as compensation gas
Combustion gas line 22.For this purpose, gas mixer according to the present invention may include by a part in combustion-supporting gas as benefit
Repay the transfer conduit that gas is transferred in combustion gas line 22.In other words, in this embodiment, in compensation gas supply pipe
At the first end on road 50, the compensation gas feeding pipe 50 can be in fluid communication with combustion gas line 22, and opposite
At two ends, compensation gas feeding pipe 50 and the combustion-supporting gas pipeline 32 are in fluid communication, thus compensation gas feeding pipe 50
Constitute the transfer conduit being transferred in combustion gas line 22 using a part in combustion-supporting gas as compensation gas.
More preferably, in the case where combustion-supporting gas is air, compensation gas may be air, therefore, directly be derived from
The compensation gas of combustion-supporting gas makes entire pipeline arrange that more flexible, space is more saved and cost is also minimized.
It is understood that such as valve not shown here or other pipelines are also in gas mixer or benefit of the invention
In the range of repaying gas supply device.
It is supplied in addition, the compensation gas feeding mechanism of equipment of the invention is constructed to be permeable to adjust to flame ionization detector
Compensation gas or other gases (i.e., sample gas, burning gases, combustion-supporting gas etc.) flow.For example, compensation gas supply dress
Set may include gas flow adjusting means 80 (for example, damper, the damping being especially located on compensation gas feeding pipe 50
Device), to facilitate the in real time or as needed flow to adjust the compensation gas for being supplied to flame ionization detector 100.
It will be understood that combustion gas line 22 and/or combustion-supporting gas pipeline 32 can also equally include gas flow adjusting means
80 (for example, it is also possible in the form of dampers).
As illustrated in fig. 1-3, the gas flow adjusting means of gas mixer are implemented as supplies positioned at the compensation gas
To at least one junction described in pipeline 50 and sample air pipe 12 and combustion gas line 22 pipe joint (for example, T-type
Pipe fitting 70) or valve (such as multiple-way valve, mechanical structure are it is known in the art that details are not described herein).But it is also contemplated that
It arrives, gas mixer of the invention may include the structure and layout of other supplied gas mixing (for example, to be mixed for accommodating
Gas, the space that separates is sealed with environment, this space respectively only with compensation gas pipeline 50 and with combustion gas line 22
Or sample air pipe 12 is connected to), rather than just pipe joint or valve.
It will further be understood that arriving, equipment of the invention can also include controller, which can be with gas source, pipe
Valve, air inlet, exhaust outlet, flow regulator in road etc. connection, with the process that entire compensation gas is supplied and it
Combustion process in flame ionization detector etc. carries out overall control/independent control afterwards.
Next, illustrating the influence using oxygen-containing gas as compensation gas to testing result in conjunction with an example.It can manage
It solves, in this example, is illustratively supplied to air as oxygen-containing gas in flame ionization detector 100, but other
The compensation gas of oxygen content is also within the scope of the invention.
It is right when burning gases are hydrogen (flow is about 30 ml/mins), the flow of sample gas is about 30 ml/min
The flow of the compensation gas as provided by compensation gas feeding mechanism (or auxiliary gas) is changed.Here, combustion-supporting gas
Preferably air, flow is about 250-300 ml/min (that is, air-fuel ratio is about 10:1), but the flow of combustion-supporting gas is to benefit
The influence for repaying the changes in flow rate of gas is smaller.
It lists in the following table, for the propane of 20 milligrams/cubic metre, when sample gas is filled the gas of nitrogen and air respectively
When bag surrounds (that is, sample gas is loaded into the gas pouch), the flow of compensation gas is initially increased to 65 ml/mins from 0, this
When the obtained variation of peak area.
It (is shown in the first three columns of following table) for the sample gas by nitrogen balance, by the peak area of empty chromatographic column
It is shown with the peak area of the specific chromatographic column (DB-624) by the applicant.It is obvious that by nitrogen balance
Sample gas in the case where, the variation of peak area caused by the compensation gas of various flows is smaller.
It (is shown in the four to six column of following table) for the sample gas by air balance, by the peak of empty chromatographic column
The peak area of the specific chromatographic column (DB-624) of area and process the applicant is shown.It is obvious that by air
In the case where the sample gas of balance, peak area caused by the compensation gas of various flows is changed greatly.
When difference between the two is 5% or so or less, the flow of compensation gas is proved can to eliminate or at least
Mitigate the oxygen in sample gas to the interference effect of testing result.For example, when the flow of compensation gas (being at this time air) is in 5cc/
When minute, 6cc/ minutes, 35cc/ minutes, 45cc/ minutes, 55cc/ minutes, 65cc/ minutes, the effect realized more meets reality
Test desired requirement.
Table 1: the testing result comparison diagram of the compensation gas under each flow
| Nitrogen balance | Peak area (empty chromatographic column) | Peak area (chromatographic column DB) | Air balance | Peak area (chromatographic column) | Peak area (chromatographic column DB) | |
| 0 | 1.518133 | 1.444347 | 0 | 1.198617 | 1.233725 | - 21.05% |
| 3.03 | 1.502016 | 1.429108 | 3.03 | 1.29696 | 1.249871 | - 13.65% |
| 4.05 | 1.503376 | 1.429911 | 4.05 | 1.324437 | 1.264058 | - 11.90% |
| 4.52 | 1.48811 | 1.413885 | 4.52 | 1.406883 | 1.275612 | - 5.46% |
| 5.05 | 1.475384 | 1.404297 | 5.05 | 1.451353 | 1.303489 | - 1.63% |
| 6.03 | 1.483733 | 1.409588 | 6.03 | 1.482165 | 1.318089 | - 0.11% |
| 7.01 | 1.494361 | 1.416005 | 7.01 | 1.58684 | 1.364741 | 6.19% |
| 15 | 1.665696 | 1.582728 | 15 | 1.989906 | 1.683565 | 19.46% |
| 25 | 1.879391 | 1.781464 | 25 | 2.099781 | 1.871345 | 11.73% |
| 35 | 1.845214 | 1.746959 | 35 | 1.925502 | 1.783859 | 4.35% |
| 45 | 1.610756 | 1.523319 | 45 | 1.604315 | 1.520916 | - 0.40% |
| 55 | 1.341518 | 1.265454 | 55 | 1.30438 | 1.249721 | - 2.77% |
| 65 | 0.923598 | 0.864705 | 65 | 0.876084 | 0.843975 | - 5.14% |
Experimental result more than being shown in detail in Fig. 5, i.e., (from 0-65 milli under each different flow of compensation gas
Liter/min) oxygen is to the annoyance level of sample gas.As described above, especially when the flow of compensation gas was 5cc/ minutes, 45cc/
Whens minute, 65cc/ minutes etc., the oxygen in sample gas can be quantized the interference effect of result.As a result, by sample gas
Deviation caused by oxygen can be modified with calculation, such as the total hydrocarbon peak area not come out with oxygen separation is not subtracted point
The oxygen peak area come is separated out, to reach more accurate analysis result.
Herein, meaning of the term " by the sample gas of nitrogen balance " in the case where sample gas is such as methane, which refers to, uses nitrogen
Methane sample gas is diluted to the concentration that experiment needs by gas.And the meaning of term " using nitrogen as sample gas " then refers to and works as pure nitrogen gas
It is analyzed as sample.In above-mentioned two situations, oxygen is not contained.
Although having references to the example of the equipment comprising flame ionization ditector 100 in the drawings to describe this hair
Bright each embodiment, it should be understood, however, that the embodiment in the scope of the present invention be also applicable to similar structure and/or
Other equipment occasions for being detected to sample gas of function, such as industrial circle, especially biologic medical field.
The description of front has been presented for many features and advantage, including various alternative embodiments and device and
The details of the structure and function of method.It is intended that it is illustrative, it is not exhaustive or restrictive.
It for those skilled in the art obviously can be to the wide in range upper of the term as expressed by appended claims
Various remodeling are made in full scope indicated by meaning, especially in structure, material, element, component, shape, size and portion
In terms of the arrangement of part, including the combination in these aspects concept described herein.These it is various remodeling without departing from
In the degree of spirit and scope of the appended claims, it is meant that they are also incorporated herein.
Claims (11)
1. a kind of equipment for being detected to sample gas, the equipment include:
Flame ionization detector (100), the flame ionization detector include sample gas import (10), combustion gas inlet
(20) and combustion-supporting gas import (30) flows into the flame ionization detector in the flame ionization detector (100)
(100) sample gas ionizes under the action of by burning gases and the flame of combustion-supporting gas generation, thus generates for institute
The signal that sample gas carries out chemical analysis is stated,
It is characterized in that, the equipment further includes compensation gas feeding mechanism, to provide benefit to the flame ionization detector
Gas is repaid, to eliminate or mitigate the interference as caused by oxygen existing for itself in the sample gas, wherein the compensation gas is
Oxygen-containing gas.
2. equipment as described in claim 1, which is characterized in that the compensation gas is air.
3. equipment as described in claim 1, which is characterized in that the equipment includes:
Sample air pipe (12), the sample air pipe are connected to the sample gas import (10)；
Combustion gas line (22), the combustion gas line are connected to the combustion gas inlet (20)；
Wherein, the compensation gas feeding mechanism includes:
Compensation gas feeding pipe (50)；
Gas mixer, the compensation gas feeding pipe (50) by the gas mixer and with the sample air pipe
(12) it is in fluid communication at least one of the combustion gas line (22), so that the compensation gas can enter the fire
It is pre-mixed before flame ionization detector (100) with corresponding gas.
4. equipment as claimed in claim 3, which is characterized in that the compensation gas feeding pipe (50) only with the sample tracheae
One of road (12) and the combustion gas line (22) are in fluid communication.
5. equipment as claimed in claim 4, which is characterized in that the compensation gas feeding pipe (50) is implemented as helps described
A part in combustion gas body is transferred to the transfer conduit in the burning gases as the compensation gas.
6. equipment as claimed in claim 2, which is characterized in that the compensation gas feeding mechanism include be constructed to be permeable to adjust to
The gas flow adjusting means of the flow of the compensation gas of the flame ionization detector supply.
7. equipment as claimed in claim 6, which is characterized in that when the flow of the sample gas is 30 ml/mins, the burning
When the flow of gas is 30 ml/min, the gas flow adjusting means are configured to adjust the flow of the compensation gas
For 5-65 ml/min, wherein the burning gases are hydrogen.
8. equipment as claimed in claim 7, which is characterized in that when the flow of the combustion-supporting gas is 250-300 ml/min
When, the gas flow adjusting means are configured to for the flow of the compensation gas to be adjusted to 5 ml/mins, 45 ml/mins
Or 65 ml/min, wherein the combustion-supporting gas is air.
9. a kind of method detected by flame ionization detector to sample gas, in the flame ionization detector
(100) in, the sample gas of the flame ionization detector is flowed into the effect by burning gases and the flame of combustion-supporting gas generation
It is lower to ionize, the signal for carrying out chemical analysis to the sample gas is thus generated,
It is characterized in that, compensation gas is provided to the flame ionization detector, to eliminate or mitigate by wrapping in the sample gas
Interference caused by the oxygen contained, wherein the compensation gas is oxygen-containing gas.
10. method as claimed in claim 9, which is characterized in that the compensation gas is in the burning gases and the sample gas
At least one of enter the flame ionization detector before be pre-mixed with it.
11. method as claimed in claim 10, which is characterized in that the combustion-supporting gas is air, and the method includes by institute
The a part stated in combustion-supporting gas is transferred in the burning gases as the compensation gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910376464.5A CN109991345A (en) | 2019-05-07 | 2019-05-07 | Equipment for being detected to sample gas and the method that sample gas is detected by flame ionization detector |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910376464.5A CN109991345A (en) | 2019-05-07 | 2019-05-07 | Equipment for being detected to sample gas and the method that sample gas is detected by flame ionization detector |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109991345A true CN109991345A (en) | 2019-07-09 |
Family
ID=67136126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910376464.5A Pending CN109991345A (en) | 2019-05-07 | 2019-05-07 | Equipment for being detected to sample gas and the method that sample gas is detected by flame ionization detector |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109991345A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110376324A (en) * | 2019-07-12 | 2019-10-25 | 北京雪迪龙科技股份有限公司 | Utilize the method and gas chromatograph of flame ionization ditector measurement oxygen concentration |
| CN110702824A (en) * | 2019-10-21 | 2020-01-17 | 江苏天瑞仪器股份有限公司 | Automatic ignition control method of hydrogen flame ionization detector |
| CN112649549A (en) * | 2020-12-21 | 2021-04-13 | 青岛明华电子仪器有限公司 | Oxygen interference compensation method for FID detector |
| CN112903879A (en) * | 2019-12-04 | 2021-06-04 | 株式会社岛津制作所 | Method and apparatus for flame ionization detection of oxygen-containing samples |
| CN114397395A (en) * | 2021-12-31 | 2022-04-26 | 杭州春来科技有限公司 | Oxygen interference correction method and system based on FID detector for non-methane total hydrocarbon determination |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3447908A (en) * | 1964-12-23 | 1969-06-03 | William Antony Wiseman | Detection systems for gas chromatography |
| US3767363A (en) * | 1970-08-06 | 1973-10-23 | Hartmann & Braun Ag | Flame ionization detection |
| JPH0720112A (en) * | 1993-07-02 | 1995-01-24 | Shimadzu Corp | Alkaline flame ionization detector |
| JPH07218490A (en) * | 1994-02-07 | 1995-08-18 | Hitachi Ltd | Gas chromatograph equipped with hydrogen flame ionization detector |
| WO1999024829A1 (en) * | 1997-11-10 | 1999-05-20 | Nguyen Huu Phuoc | Apparatus and method for gas phase chromatography |
| CN105067730A (en) * | 2015-07-30 | 2015-11-18 | 安徽中杰信息科技有限公司 | Hydrogen flame ionization detector for carrying out quantitative analysis on hydrocarbon mixture |
| CN210142107U (en) * | 2019-05-07 | 2020-03-13 | 赛默飞世尔（上海）仪器有限公司 | A equipment for sample gas detects |
-
2019
- 2019-05-07 CN CN201910376464.5A patent/CN109991345A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3447908A (en) * | 1964-12-23 | 1969-06-03 | William Antony Wiseman | Detection systems for gas chromatography |
| US3767363A (en) * | 1970-08-06 | 1973-10-23 | Hartmann & Braun Ag | Flame ionization detection |
| JPH0720112A (en) * | 1993-07-02 | 1995-01-24 | Shimadzu Corp | Alkaline flame ionization detector |
| JPH07218490A (en) * | 1994-02-07 | 1995-08-18 | Hitachi Ltd | Gas chromatograph equipped with hydrogen flame ionization detector |
| WO1999024829A1 (en) * | 1997-11-10 | 1999-05-20 | Nguyen Huu Phuoc | Apparatus and method for gas phase chromatography |
| CN105067730A (en) * | 2015-07-30 | 2015-11-18 | 安徽中杰信息科技有限公司 | Hydrogen flame ionization detector for carrying out quantitative analysis on hydrocarbon mixture |
| CN210142107U (en) * | 2019-05-07 | 2020-03-13 | 赛默飞世尔（上海）仪器有限公司 | A equipment for sample gas detects |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110376324A (en) * | 2019-07-12 | 2019-10-25 | 北京雪迪龙科技股份有限公司 | Utilize the method and gas chromatograph of flame ionization ditector measurement oxygen concentration |
| CN110702824A (en) * | 2019-10-21 | 2020-01-17 | 江苏天瑞仪器股份有限公司 | Automatic ignition control method of hydrogen flame ionization detector |
| CN112903879A (en) * | 2019-12-04 | 2021-06-04 | 株式会社岛津制作所 | Method and apparatus for flame ionization detection of oxygen-containing samples |
| JP2021089268A (en) * | 2019-12-04 | 2021-06-10 | 株式会社島津製作所 | Method and device for detecting ionization of hydrogen flames for oxygen-containing sample |
| JP7380480B2 (en) | 2019-12-04 | 2023-11-15 | 株式会社島津製作所 | Hydrogen flame ionization detection method and device for samples containing oxygen |
| CN112903879B (en) * | 2019-12-04 | 2024-06-07 | 株式会社岛津制作所 | Method and device for flame ionization detection of oxygen-containing samples |
| CN112649549A (en) * | 2020-12-21 | 2021-04-13 | 青岛明华电子仪器有限公司 | Oxygen interference compensation method for FID detector |
| CN114397395A (en) * | 2021-12-31 | 2022-04-26 | 杭州春来科技有限公司 | Oxygen interference correction method and system based on FID detector for non-methane total hydrocarbon determination |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109991345A (en) | Equipment for being detected to sample gas and the method that sample gas is detected by flame ionization detector | |
| JP6461254B2 (en) | Gas injection system for isotope ratio analyzer and method for determining isotope ratio | |
| CN102998362B (en) | The Field adjustment of mass spectrometer system | |
| JP3607997B2 (en) | Analyzer for trace impurities in gas | |
| CN109490443A (en) | A kind of non-methane total hydrocarbons content detection device and method | |
| CN106064026A (en) | Multicomponent gas mixing system | |
| CN105987967B (en) | Non-methane total hydrocarbons and benezene material detect dedicated unit | |
| CN204479528U (en) | NMHC and benzene class material detect special purpose device | |
| CN108226268A (en) | Gas analyzing apparatus, gas sampling device and analysis method for gases | |
| WO2022221033A3 (en) | System and method for dual bio-sensor fabrication and use | |
| CN214278048U (en) | double-FID detection device for analyzing methane and non-methane total hydrocarbons | |
| US20190162636A1 (en) | Process and device for diluting an aerosol | |
| CN210142107U (en) | A equipment for sample gas detects | |
| US20080168752A1 (en) | Separating particulate-containing gas flow into particulate and non-particulate flow portions | |
| TW550384B (en) | Method and apparatus for analyzing impurities in gases | |
| JP2006502532A (en) | Method and apparatus for performing ion mobility spectrometry | |
| GB2513120A (en) | Method of determining an isotope ratio | |
| CN117054511B (en) | Non-methane total hydrocarbon detection device and method based on double detectors | |
| CN212845223U (en) | Sensitivity compensation device for hydrogen flame ionization detector | |
| CN218917295U (en) | System for be used for trace gas impurity analysis in silane gas | |
| US6107805A (en) | Extended detection zone in an ionization detector | |
| CN210572155U (en) | Air quality monitoring system | |
| CN219122123U (en) | Detection device | |
| JP2004061321A (en) | Method and apparatus for analyzing a very small quantity of impurity in gas | |
| JP3789093B2 (en) | Hydrogen concentration measuring device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |