CN106124663B - A kind of detection method of Carbon Dioxide in Air content - Google Patents
A kind of detection method of Carbon Dioxide in Air content Download PDFInfo
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- CN106124663B CN106124663B CN201610614477.8A CN201610614477A CN106124663B CN 106124663 B CN106124663 B CN 106124663B CN 201610614477 A CN201610614477 A CN 201610614477A CN 106124663 B CN106124663 B CN 106124663B
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- 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
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- 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
- G01N30/66—Thermal conductivity detectors
Abstract
The present invention discloses a kind of detection method of Carbon Dioxide in Air content, and this method comprises the following steps: the carbonated mixed gas in acquisition monitoring region;Carbon dioxide is isolated from the carbonated mixed gas;The carbon dioxide isolated is detected to obtain detection data;The detection data is acquired and handled, obtains the carbon dioxide content of carbonated mixed gas in monitoring region.This method detection sensitivity is high, and detection data can retain for a long time, meets the requirement that laboratory testing is traced to the source.
Description
Technical field
It the present invention relates to the use of the technical field of chromatography detection gas content.More particularly, in a kind of air two
The detection method of content of carbon oxide.
Background technique
Titanium dioxide Carbon analysis is the common evaluation index of occupational health and public places sanitary situation, is also used for anoxic and stops up
Cease the detection of accident emergency rescue site.
The country, which uses, at present is not divided infrared carbon dioxide direct-reading determining instrument measuring method.The original of this method measurement
Reason is using carbon dioxide to the selective absorption of the infrared ray of specific wavelength.In a certain range, absorption value and dioxy
It is in a linear relationship to change concentration of carbon.The concentration of carbon dioxide in sample is determined according to absorption value.Discovery measurement scene in real work
Vapor have interference effect to measurement.The direct-reading instrument that majority uses can not retain Original Analytical Data, not be able to satisfy measurement
Initial data is traced to the source problem.
It is external at present to use method for chromatographic determination, it is measured using portable gas-chromatography instrument, analysis chromatographic column uses
1.5*6mm 80/100mesh Poropk QS separates carbon dioxide.Detect model 500-15000ppm (900mg/m3-27000mg/
m3).But this chromatographic higher cost is not suitable for using in China, thus, explore the chromatograph for being suitble to China application
Detection method is significantly.
Summary of the invention
It is an object of the present invention to provide a kind of detection sides of carbonated carbon dioxide in gas mixture content
Method, this method detection sensitivity is high, and detection data can retain for a long time, meets the requirement that laboratory testing is traced to the source.
In order to achieve the above objectives, the present invention adopts the following technical solutions:
A kind of detection method of Carbon Dioxide in Air content, described method includes following steps:
1) the carbonated mixed gas in acquisition monitoring region;
2) carbon dioxide is isolated from the carbonated mixed gas;
3) simultaneously acquisition testing data detect to the carbon dioxide isolated;
4) detection data is handled, obtains the carbon dioxide content of carbonated mixed gas in monitoring region.
Preferably, the content range of step 1) the carbonated carbon dioxide in gas mixture is 588mg/m3-
35280mg/m3。
Preferably, the step 2) carbon dioxide of isolating from carbonated mixed gas includes using gas chromatograph
Isolate carbon dioxide.
Preferably, it includes being detected with thermal conductivity detector (TCD) that described pair of the step 3) carbon dioxide isolated, which carries out detection,.
Preferably, step 4) the processing detection data includes being adopted with chromatographic work station to the detection data
Collection and processing obtain the carbon dioxide content of carbonated mixed gas in monitoring region.
Preferably, the chromatographic condition of the gas chromatograph are as follows: 1.5-2.0m*3-4mm stainless steel or glass column;
Preferably, the silica gel of filling 60-80 mesh or 80-100 mesh in the chromatographic column;Carrier gas used is helium, described
The flow of carrier gas is 25-35ml/min;
Preferably, the column temperature of the chromatographic column is 45-65 DEG C, and the gasification room temperature of the chromatographic column is 45-65 DEG C, described
It is 45-65 DEG C that chromatographic column, which detects room temperature,.
Preferably, the bridge current when thermal conductivity detector (TCD) is detected is 160-200mA.
Preferably, the method further includes the draftings of standard curve.
Preferably, the drafting of the standard curve specifically comprises the following steps:
A. prepare the calibrating gas sample of more parts of different carbon dioxide contents;
B. every part of calibrating gas sample is obtained into the average peak of every part of calibrating gas sample respectively to gas chromatograph sampling
High and average peak area;
C. carbon dioxide content is made using the peak height average value of every part of obtained standard sample or peak area average value
Standard curve, while obtaining linear regression equation.
Preferably, carbon dioxide content is respectively as follows: 588mg/m in calibrating gas sample described in step A3、1176mg/m3、
2352mg/m3、4704mg/m3、9408mg/m3、18816mg/m3、35280mg/m3;
Sample introduction described in step B is at least continuous 3 sample introductions, and the sample volume of each sample introduction is 3mL;
Linear regression equation described in step C are as follows: y=ax+b, wherein x is the content of carbon dioxide, and y is peak height average value
Or peak area average value, a and b are the slope and intercept of the standard curve.
Beneficial effects of the present invention are as follows:
1. current country's vocational health and public place titanium dioxide Carbon analysis, application is not to be divided infrared direct-reading instrument
Measuring method.Scene vapor has an interference to measurement when this method measures, and most direct-reading Instrument measurings cannot retain it is original
Determination data, is unfavorable for the requirement that laboratory is traced to the source, and this method can make up its defect;
2. this method chromatographic column cost is lower than external existing detection method and can be parsed into activated Reusability saving
This;
3. since this method optimizes carrier gas flux 3/4 helium can be saved compared with foreign method;
4. the minimum concentration out that this method measures carbon dioxide is 92ppm (180mg/m3), a little higher than state of detection sensitivity
The concentration limit (156ppm) of outer detection method;
It can use the existing chromatograph of testing agency, be not required to increase and purchase instrument and equipment, favorably reduce testing cost.
5. chromatographic column of the present invention use common desktop chromatograph, 1.5*3mm60/80 mesh silica gel post separation carbon dioxide,
Determining instrument and chromatographic column cost are reduced, detection range has reached 588mg/m3- 35280mg/m3, the chromatographic column that uses herein
It can be by activating Reusability.And new chromatographic column is needed replacing after the external chromatography aging of column used.
Since daily measurement carbon dioxide content is often less than 5000mg/m3, and anoxia asphyxia ambient carbon dioxide content
10000mg/m can be reached3More than.So the present invention devises low concentration measurement standard curve and high concentration measures standard curve
Method, for it is different need using.
The present invention is by carbon dioxide content in 588mg/m3-4704mg/m3Between be defined as low concentration, carbon dioxide content
In 4704mg/m3-35280mg/m3Between be defined as high concentration.
Low concentration canonical plotting is shown in Fig. 1, and high standard curve graph is shown in Fig. 2
Detailed description of the invention
Fig. 1 is low concentration canonical plotting;
Fig. 2 is high standard curve graph;
Fig. 3 is that 300ppm carbon dioxide Standard Gases analyze chromatogram;
Fig. 4 is carboloy dioxide analysis chromatogram in 1 outside atmosphere of embodiment;
Fig. 5 is the real-time experimental data of 1 chromatogram of embodiment;
Fig. 6 is carboloy dioxide analysis chromatogram in 2 room air of embodiment;
Fig. 7 is the real-time experimental data of 2 chromatogram of embodiment;
Fig. 8 is that 3 soft berth sleeper Carbon Dioxide in Air of embodiment analyzes chromatogram;
Fig. 9 is the real-time experimental data of 3 chromatogram of embodiment.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
A kind of detection method of carbonated carbon dioxide in gas mixture content of the present invention is to utilize gas chromatograph
Carbon dioxide in mixed gas is separated, then detects the carbon dioxide isolated by thermal conductivity detector (TCD),
And the data that will test are transmitted to chromatographic work station, and collected detection data is recorded and handled by chromatographic work station,
Chromatogram is drawn out, it is qualitative by the carbon dioxide retention time progress in chromatogram, it is quantified by peak height or peak area,
Finally obtain carbon dioxide in gas mixture content.
The method of the present invention specifically comprises the following steps:
A kind of detection method of carbonated carbon dioxide in gas mixture content, the method for the present invention are suitable for detection two
Content of carbon oxide is in 588mg/m3-35280mg/m3Carbon dioxide content in the carbonated mixed gas of range;This method
Include the following steps:
1) with the carbonated mixed gas in aluminium foil sampler bag acquisition monitoring region;
2) carbon dioxide is isolated from carbonated mixed gas with gas chromatograph;
3) carbon dioxide isolated is detected with thermal conductivity detector (TCD);
4) with chromatographic work station acquisition and processing detection data, two of carbonated mixed gas in monitoring region are obtained
Content of carbon oxide.
The chromatographic condition of gas chromatograph are as follows: 1.5-2.0m*3-4mm stainless steel chromatographic column;60- is filled in the chromatographic column
The silica gel of 80 mesh or 80-100 mesh;Carrier gas used is helium, and the flow of the carrier gas is 25-35ml/min;The chromatographic column
Column temperature be 45-65 DEG C, the gasification room temperature of the chromatographic column is 45-65 DEG C, and the chromatographic column detection room temperature is 45-65
℃。
Bridge current when thermal conductivity detector (TCD) is detected is 160-200mA.
This method further comprises the drafting of standard curve, is specifically comprised the following steps:
A. prepare the more parts of calibrating gas samples for containing different carbon dioxide contents respectively;
B. every part of calibrating gas sample is obtained into the peak height and peak area of every part of sample to gas chromatograph continuous sample introduction;
C. using the peak height average value or peak area average value of every part of obtained calibrating gas sample feeding to corresponding dioxy
Change carbon content progress linear regression and obtains linear regression equation.
Carbon dioxide content described in step A is respectively as follows: 588mg/m3、1176mg/m3、2352mg/m3、4704mg/m3、
9408mg/m3、18816mg/m3、35280mg/m3;
The continuous sample introduction of step B is at least continuous 3 sample introductions, and the sample volume of each sample introduction is 3mL;
The linear regression equation of step C are as follows: the linear regression equation of low concentration of carbon dioxide is y=0.5233x+
23.043;The linear regression equation of high concentration carbon dioxide are as follows: y=0.4917x-156.54.
Following methods can be selected to the acquisition of tested gas:
The sampling pump that can control sampling quantity can be used in sampling, and medical bigeminy ball or 100ml glass note also can be used
Emitter;Sampling pump or medical bigeminy ball acquisition gas be stored in sampler bag, sampler bag have sealing-plug thus can seal
It saves, the silica gel seal of tube can be used in syringe;About the amount of acquisition gas, the gas of acquisition is controlled in sampler bag capacity
80%, syringe reaches 100ml when sampling and also complies with custom requirements.
The separation principle of carbon dioxide: silica gel is a kind of porosity object formed by poly silicic acid through intramolecular dehydration
Matter, chemical composition are as follows: SiO2·×H2O belongs to indefiniteness structure.The basic structure particle of silica gel be Si-O tetrahedron, be by
Si-O tetrahedron mutually accumulates the skeleton for forming silica gel.When accumulation, the space in particle is the gap of silica gel.
Since silica gel is porous material, there is biggish specific surface area, and the hydroxyl on surface is with a degree of
Polarity energy Preferential adsorption polar molecule.
Although carbon dioxide is nonpolar molecule, since its internal carbon-oxygen bond has polar molecule characteristic.Therefore silicon
Glue has suction-operated to carbon dioxide, and oxygen and nitrogen are nonpolar molecule.
Above-mentioned difference of this technology based on oxygen, nitrogen, carbon dioxide in sample, completes carbon dioxide using silica gel
Separation.Carbon dioxide is long compared with the retention time of oxygen, nitrogen on a silica gel column, and this technology can accomplish that oxygen and nitrogen occur one
There is a single chromatographic peak, preferably meet the purpose of carbon dioxide separation in secondary colour spectral peak, carbon dioxide.
Fig. 3 be using the method for the present invention to carbon dioxide content be 300ppm mixed gas in carbon dioxide gas into
The isolated carbon dioxide separation chromatogram of row, the figure illustrate that this method can isolate carbon dioxide from mixed gas,
Qualitative and quantitative analysis can be carried out to the carbon dioxide in normal atmosphere, since it is desired that titanium dioxide in the place of measurement carbon dioxide
Carbon content is typically greater than 300ppm.
The chromatographic isolation degree (R) of carbon dioxide of the present invention:
Chromatographic isolation degree refers to the difference of the retention time at adjacent two peak and the ratio of average peak width.Also it is resolution ratio, is indicated
The separation degree at adjacent two peak.R is bigger, shows that two adjacent groups point separation is better.Generally as R < 1, two peaks overlap;
As R=1.0, separating degree is up to 98%;As R=1.5, separating degree is up to 99.7%.Usually use R=1.5 as adjacent two
The mark that component has been kept completely separate.As R=1, referred to as 4 σ separation, two peaks are basically separated, and exposed peak area is 95.4%, inside
Peak base weight folded about 2%.When R=1.5, referred to as 6 σ separation, exposed peak area is 99.7%.R >=1.5 are known as being kept completely separate." China
Pharmacopeia " regulation R should be greater than 1.5.
Separating degree calculation formula: R=2 (tR2-tR1)/(W1+W2);
R: chromatographic isolation degree;
tR2: the retention time (min) at latter peak in adjacent two peak;
tR1: the retention time (min) at previous peak in adjacent two peak;
W1、W2: the peak width (min) at this adjacent two peak;
It is a chromatographic peak appearance since oxygen and nitrogen cannot separate on a silica gel column, but carbon dioxide energy and oxygen
It is sufficiently separated with nitrogen.Therefore emphasis of the present invention considers oxygen+nitrogen chromatographic peak and carbon dioxide separating capacity;
Experimental data:
tRCarbon dioxide=0.458;tROxygen+nitrogen=0.159;Peak widthOxygen+nitrogen=7mm;Peak widthCarbon dioxide=10mm;
Chart speed=69mm/min (0.01449min/mm);
R=2 (0.458-0.159)/(7*0.01449)+(10*0.1449)
=2.4;
It can be seen that chromatographic isolation degree R=2.4 of the present invention meets the requirement of aforementioned R > 1.5, be analyzed sample chromatogram peak with
Adjacent chromatographic peak is kept completely separate.
The characteristic that thermal conductivity detector (TCD) with different thermal conductivities, heated filament there is resistance to vary with temperature based on gas with various,
Isolate through molecular sieve column two are completed using four resistance walls (the rhenium tungsten resistance) heat balance principle of classical " resistance bridge "
The electric signal convert task of carbonoxide.
Chromatographic work station work station be N2000 type, be by its hardware and software cooperate complete chromatographic data acquisition,
For record to provide analysis chromatogram, chromatogram be used to mark the retention time chromatographic peak area of analyte, Jin Erda
To carrying out qualitative and quantitative purpose to analyte.
Embodiment 1
The measurement of carbon dioxide content in outside atmosphere:
1. experiment equipment: carbonated amount are as follows: 588mg/m3、1 176mg/m3、2 352mg/m3、4704mg/m3Mark
Quasi- gas, high-purity helium, 60/80 mesh silica gel, volume 500ml aluminium foil sampler bag, six-way valve match 3ml gasometry pipe,
SP2100 gas chromatograph, TCD, chromatographic work station N2000 type;
2. sampling: there is no motor vehicle activity venue in outdoor ward, within the scope of the stance breathing zone of people, repeatedly
Squeeze medical bigeminy ball is inflated to gas production bag body product into aluminium foil sampler bag 80% or so.Then remove bigeminy from gas production bag
Ball squeezes the gas for excluding to acquire in gas production bag, repeatedly for three times.Finally with bigeminy ball gas production to 80% or so of sampler bag volume
Lab analysis is taken back into sampler bag sealing with the sealing valve of sampler bag;
3. adjusting gas chromatograph, the analysis condition of gas chromatograph are as follows: column length 1.5m, internal diameter 3mm inside fill out 60/
80 mesh silica gel, 50 degree of column temperature, 50 degree of detector, thermal conductivity electric bridge 181mA, carrier gas is helium, helium gas flow 25ml/min;
4. drawing standard curve preparation:
Taking carbon dioxide content respectively is 588mg/m3, 1176mg/m3, 2352mg/m3, 4704mg/m3Calibrating gas,
Calibrating gas is accommodated in gas production bag, gas production bag passes through six-way valve and chromatographic injection port connection, the standard of every kind of content
Gas three times, corresponds to oxygen content with the mean value of peak area three times from injection port sample introduction, carries out linear regression and obtains concentration two
Carbonoxide standard curve, it is carboloy dioxide analysis chromatogram in the present embodiment outside atmosphere that the data of standard curve, which are shown in Table 1, Fig. 4,;
Fig. 5 is the real-time experimental data of the present embodiment chromatogram;
Table 1
5. sample to be tested detects: under above-mentioned instrument condition, after chromatograph baseline straightening, the sample sack of acquisition being passed through
Six-way valve is connected to chromatographic injection port, and sample introduction 3ml under test gas, the peak area for measuring carbon dioxide under test gas is 396;
6. calculating: according to linear regression equation, y=0.5233x+23.043 substitutes into peak area value y=396, acquire to
Survey carbon dioxide in gas content x value is 712.7mg/m3。
This measurement result can be scaled in 363.6ppm and normal atmosphere carbon dioxide content 350ppm extremely
Report between 400ppm is consistent.
Embodiment 2
The measurement of carbon dioxide content in room atmosphere:
1. experiment equipment: carbonated amount are as follows: 588mg/m3、1 176mg/m3、2 352mg/m3、4 707mg/m3's
Calibrating gas, high-purity helium, 60/80 mesh silica gel, volume 500ml aluminium foil sampler bag, six-way valve match 3ml gasometry pipe,
SP2100 gas chromatograph, TCD, chromatographic work station N2000 type;
2. sampling: in 30m2Laboratory within the scope of the sitting posture breathing zone of people, repeatedly extrudes medical after 3 manually make 6h
Bigeminy ball is inflated to 80% or so of gas production bag body product into aluminium foil sampler bag.Then remove bigeminy ball from gas production bag, the row of extruding
Except the gas acquired in gas production bag, repeatedly for three times.Finally sampler bag is used with bigeminy ball gas production to 80% or so of sampler bag volume
Sealing valve sampler bag is sealed after in lab analysis;
3. adjusting gas chromatograph, the analysis condition of gas chromatograph are as follows: column length 1.5m, internal diameter 3mm inside fill out 60/
80 mesh silica gel, 50 degree of column temperature, 50 degree of detector, thermal conductivity electric bridge 181mA, carrier gas is helium, helium gas flow 25ml/min;
4. drawing standard curve preparation:
Taking carbon dioxide content respectively is 588mg/m3, 1176mg/m3, 2352mg/m3, 4704mg/m3Calibrating gas,
Calibrating gas is accommodated in gas production bag, gas production bag passes through six-way valve and chromatographic injection port connection, the standard of every kind of content
Gas three times, corresponds to carbon dioxide content with the mean value of peak area three times, progress linear regression obtains low dense from injection port sample introduction
Carbon dioxide standard curve is spent, it is carboloy dioxide analysis color in the present embodiment room air that the data of standard curve, which are shown in Table 2, Fig. 6,
Spectrogram;Fig. 7 is the real-time experimental data of the present embodiment chromatogram;
Table 2
5. sample to be tested detects: under above-mentioned instrument condition, after chromatograph baseline straightening, the sample sack of acquisition being passed through
Six-way valve is connected to chromatographic injection port, and sample introduction 3ml under test gas, the peak area for measuring carbon dioxide under test gas is 968;
6. calculating: according to linear regression equation, y=0.5233x-23.043 substitutes into peak area value y=968, acquire to
Survey carbon dioxide in gas content x value is 1893.8mg/m3。
China workplace carbon dioxide content limit value is 9000mg/m3, this measurement result complies with the national standard requirements.
Embodiment 3
The measurement of carbon dioxide content in train soft berth sleeper:
1. experiment equipment: carbonated amount are as follows: 4704mg/m3, 9408mg/m3, 18816mg/m3, 35280mg/m3's
Calibrating gas, high-purity helium, 60/80 mesh silica gel, volume 500ml aluminium foil sampler bag, six-way valve match 3ml gasometry pipe,
SP2100 gas chromatograph, TCD, chromatographic work station N2000 type;
2. sampling: after 4 people's seat soft berth sleepers drive a vehicle 4h, within the scope of the sitting posture breathing zone of people, repeatedly extruding medical
Bigeminy ball is inflated to 80% or so of gas production bag body product into aluminium foil sampler bag.Then remove bigeminy ball from gas production bag, the row of extruding
Except the gas acquired in gas production bag, repeatedly for three times.Finally sampler bag is used with bigeminy ball gas production to 80% or so of sampler bag volume
Sealing valve by sampler bag sealing take back lab analysis;
3. adjusting gas chromatograph, the analysis condition of gas chromatograph are as follows: column length 1.5m, internal diameter 3mm inside fill out 60/
80 mesh silica gel, 50 degree of column temperature, 50 degree of detector, thermal conductivity electric bridge 181mA, carrier gas is helium, helium gas flow 25ml/min;
4. drawing standard curve preparation:
Taking carbon dioxide content respectively is 4707mg/m3, 9408mg/m3, 18816mg/m3, 35280mg/m3Standard Gases
Calibrating gas is accommodated in gas production bag by body, and gas production bag passes through six-way valve and chromatographic injection port connection, the mark of every kind of content
Quasi- gas three times, corresponds to carbon dioxide content with the mean value of peak area three times from injection port sample introduction, carries out linear regression and obtains height
Concentration carbon dioxide standard curve, it is the present embodiment soft berth sleeper Carbon Dioxide in Air that the data of standard curve, which are shown in Table 3, Fig. 8,
Analyze chromatogram;Fig. 9 is the real-time experimental data of the present embodiment chromatogram;
Table 3
5. sample to be tested detects: under above-mentioned instrument condition, after chromatograph baseline straightening, the sample sack of acquisition being passed through
Six-way valve is connected to chromatographic injection port, and sample introduction 3ml under test gas, the peak area for measuring oxygen under test gas is 3698;
6. calculating: according to linear regression equation, y=0.4917x-156.54 enters peak area value y=3698, acquire to
Survey carbon dioxide in gas content x value is 7839.2mg/m3。
The calibrating gas used in various embodiments of the present invention is the mixed gas of carbon dioxide and nitrogen.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (7)
1. a kind of detection method of Carbon Dioxide in Air content, which is characterized in that described method includes following steps:
1) the carbonated mixed gas in acquisition monitoring region;
2) carbon dioxide is isolated from the carbonated mixed gas;
3) carbon dioxide isolated is detected to obtain detection data;
4) it acquires and handles the detection data, obtain carbonated carbon dioxide in gas mixture content in monitoring region;
The content range of the step 1) carbonated carbon dioxide in gas mixture is 588mg/m3- 35280mg/m3;
It includes isolating dioxy with gas chromatograph that the step 2 isolates carbon dioxide from carbonated mixed gas
Change carbon;
The chromatographic condition of the gas chromatograph are as follows: 1.5-2.0m × 3-4mm stainless steel or glass column;In the chromatographic column
Fill the silica gel of 60-80 mesh or 80-100 mesh;Carrier gas used is helium, and the flow of the carrier gas is 25-35ml/min;It is described
The column temperature of chromatographic column is 45-65 DEG C, and the gasification room temperature of the gas chromatograph is 45-65 DEG C, the inspection of the gas chromatograph
Surveying room temperature is 45-65 DEG C.
2. detection method according to claim 1, which is characterized in that pair carbon dioxide isolated described in step 3) carries out
Detection includes being detected with thermal conductivity detector (TCD).
3. detection method according to claim 1, which is characterized in that acquired described in step 4) and handle the detection data
Including the detection data is acquired and is handled with chromatographic work station, carbonated mixed gas in monitoring region is obtained
Middle carbon dioxide content.
4. detection method according to claim 2, which is characterized in that the electric bridge electricity when thermal conductivity detector (TCD) is detected
Stream is 160-200mA.
5. detection method according to claim 1, which is characterized in that the method further includes drawing for standard curve
System.
6. detection method according to claim 5, which is characterized in that the drafting of the standard curve specifically includes following step
It is rapid:
A. prepare the calibrating gas sample of more parts of different carbon dioxide contents;
B. every part of calibrating gas sample is obtained into the peak height and peak face of every part of calibrating gas sample respectively to gas chromatograph sampling
Product;
C. standard is made to carbon dioxide content using the peak height average value of every part of obtained standard sample or peak area average value
Curve, while obtaining linear regression equation.
7. detection method according to claim 6, it is characterised in that: carbon dioxide in calibrating gas sample described in step A
Content be respectively as follows: 588mg/m3,1176mg/m3,2352mg/m3,4704mg/m3,9408mg/m3,18816mg/m3,
35280mg/m3;Sample introduction described in step B is at least continuous 3 sample introductions, and the sample volume of each sample introduction is 3mL;Straight line described in step C
Regression equation are as follows: y=ax+b, wherein x is the content of carbon dioxide, and y is peak height average value or peak area average value, and a and b are
The slope and intercept of the standard curve.
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