CN110487927A - The measuring method of methanol in a kind of exhaust of solid pollution source - Google Patents
The measuring method of methanol in a kind of exhaust of solid pollution source Download PDFInfo
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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
- G01N30/04—Preparation or injection of sample to be analysed
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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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
- G01N30/26—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
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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
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
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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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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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
- G01N30/26—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
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Abstract
The invention discloses the measuring methods of methanol in a kind of exhaust of solid pollution source, it include: sample acquisition, sample treatment, the preparation of calibrating gas, the production of standard curve and the several steps of measurement, wherein sample acquisition includes sampling in a organized way, inorganization sampling and blank sample sampling；Sample treatment takes the sample gas being stored in aluminium foil bag or 100ml syringe with 1ml syringe, after replacing 3 times repeatedly, 1.0ml sample gas is taken to be analyzed；The gas phase condition of gas chromatograph is set as using PEG-20M capillary chromatographic column 30m*0.50mm*1.0um in determination step, and column temperature is 70 degree, and temperature of vaporization chamber is 200 degree, and detection room temperature is 230 degree, carrier gas flux 10ml/min.Carbinol compound result detection data is accurate in method detection solid pollution source exhaust of the invention, meets national requirements, time-saving and efficiency.
Description
Technical field
The present invention relates to the measuring methods of methanol in a kind of exhaust of solid pollution source, belong to compound field of chemical detection.
Background technique
For in the measurement of surrounding air noxious material, gas is usually used in the detection method of methanol in the exhaust of solid pollution source
Phase chromatography, requirements of the national standard solid pollution source exhaust in methanol measurement tune part be 2m × 2~3mm glass (or stainless steel)
Packed column, chromatography column packings: 80~120 mesh of 5%Carbowax 20M Carbopack B, column temperature: 70 degree；Vaporize room temperature
Degree: 200 degree；Detection room temperature: 230 degree；Carrier gas (nitrogen) flow: 32ml/min.Likewise, having for other class surrounding airs
Gas chromatography can also be used in the measurement of noxious material, core technology is that selection uses suitable chromatographic column and suitable column
Temperature, temperature of vaporization chamber, detection room temperature and carrier gas flux.If groped less than suitable condition, will not appearance or appearance not
Accuracy completely to influence detection data.
For numerous projects detected using gas chromatography, required according to standard requirements disparity items using different
Chromatographic column frequently replaces chromatographic column thus and leads to the risk for occurring increasing pillar damage.One expensive (the hair of root chromatogram column price
Tubule about more than 3000 yuan one) and it is replaced as frequently as the damage that pillar easily causes pillar, and also it is time-consuming.
Therefore selection how uses a capillary column, is applicable in the condition of the measurement of methanol in the exhaust of solid pollution source,
And ensure that every detection data is accurate and meets the requirements, accomplish to save time saving and data accurately multiple advantage, is current
Researcher's urgent need to solve the problem in detection industry.
Summary of the invention
Goal of the invention: the present invention aiming at the shortcomings in the prior art, provides the dense of methanol in a kind of exhaust of solid pollution source
Detection method is spent, there is cost to reduce, saves time, the high advantage of accuracy.
Technical solution: the measuring method of methanol in a kind of solid pollution source exhaust of the present invention includes the following steps:
(1) sample acquires: including sampling in a organized way, inorganization sampling and blank sample sampling；The inorganization sampling exists
Sampled point scene, after first washing sampling syringe 5-6 times repeatedly, pumps full live air, rapid sealing injection device mouth takes back reality
Test room analysis；Organized sampling is protruded into exhaust tube sampled point in the sampling appropriate mineral wool of tube head plug, starting pumping
Pump, sampling system pipeline is sufficiently cleaned, then twitch syringe with the gas in exhaust tube first, after washing 5-6 times repeatedly,
The gas of required volume is pumped full, and is sealed with rubber cap rapidly, laboratory is taken back；The blank sample is sampled as syringe band
To sampled point, in addition to being not connected to samplers sample air sample, remaining operates same sample；
(2) sample treatment: the sample gas being stored in aluminium foil bag or 100ml syringe is taken with 1ml syringe, is replaced repeatedly
After 3 times, 1.0ml sample gas is taken to be analyzed, it, can be with after cleaned air or high pure nitrogen dilution if concentration is more than measurement range
Measurement, multiplied by extension rate when calculating；
(3) preparation of calibrating gas: being diluted distribution with 100ml all-glass syringe as needed, takes methanol standard
Gas, according to the concentration of sample to be tested, in the range of linearity 5.0-1.0*10 of methanol4mg/m3It is interior dilute with cleaned air or high pure nitrogen
Release the standard series for being configured to 15.8ug/l, 39.6ug/l, 79.2ug/l, 158.4ug/l concentration；
(4) gas chromatograph the production and measurement of standard curve: is adjusted to optimum determining state, sample introduction 1.0ml, measurement
Each standard series, each concentration replication 3 times, the peak height for measuring each concentration of standard series respectively or peak area mean value are to corresponding
Methanol standard gas concentration draw standard curve or calculate regression equation.
Further, in the sampling of step (1) inorganization if necessary, sample gas can be repeatedly washed with syringe, is infused
After entering bladder tank, laboratory is taken back.
Further, rubber cap is lined with polytetrafluoroethylene film in step (1).
Further, the gas phase condition of gas chromatograph is set as using PEG-20M capillary in step (4) determination step
Chromatographic column 30m*0.50mm*1.0um, column temperature are 70 degree, and temperature of vaporization chamber is 200 degree, and detection room temperature is 230 degree, carrier gas stream
Amount is 10ml/min.
Further, step (4) measurement includes sample measurement and reference substance measurement, and the reference substance is measured as measurement blank
Cleaned air is compareed, peak height or peak area value are obtained；The sample is measured as the similarity condition measurement sample with measurement standard series
Product gas obtains sample by standard curve after the sample peak height or peak area value measured subtracts blank control peak height or peak area value
The concentration of middle methanol.
The utility model has the advantages that beneficial effects of the present invention are as follows:
(1) in this solid pollution source exhaust of the invention methanol measuring method, using PEG-20M capillary chromatography
Column, column temperature are 70 degree, and 200 degree of temperature of vaporization chamber, detection room temperature is 230 degree, carrier gas flux 10ml/min, and detection solid is dirty
Carbinol compound result detection data is accurate in the exhaust of dye source, meets national requirements, time-saving and efficiency；
(2) this PEG-20M capillary column is selected, after setting suitable determination condition, while alcohols can also be carried out
The detection for closing other compounds in object solves the problems, such as to be replaced as frequently as pillar and easily causes the damage of pillar and time-consuming, both saved
The about time saving accuracy that more importantly ensure that data again；
(3) preparation of standard gas is reduced the usage amount of standard gas using improved method of the invention, for
Guarantee that the preci-sion and accuracy of sample measurement plays good facilitation.
Specific embodiment
The present invention is further explained in the light of specific embodiments:
Embodiment 1
Using the detection method of methanol in gas chromatography measurement solid pollution source exhaust:
1, instrument
A) organized emission monitoring sampling instrument: with reference to 9.3 configuration sampling system in GB16157-1996.
B) sampling pipe: with the materials in the tube of the stainless steel of appropriate size, hard glass or polytetrafluoroethylene (PTFE) material, and with can add
The insulation jacket of temperature to 120 DEG C or more.
C) sampler: 100ml all-glass syringe.
D) flow measurement device: with reference to 9.3.6 in GB16157-1996.
E) aspiration pump: with reference to 9.3.7 in GB16157-1996.
F) connecting tube: the silicone rubber tube of teflon hose or inner liner polytetrafluoroethylene film.
G) uncontrollable discharge monitors sampling instrument: 100ml all-glass syringe.
H) bladder tank: aluminium foil laminated film airbag.
I) syringe, 1.0ml.
J) gas chromatograph: day beauty 7900II.
2, instrument testing conditions:
PEG-20M capillary chromatographic column.
[a] column temperature is 70 degree.
[b] temperature of vaporization chamber is 200 degree.
It is 230 degree that [c], which detects room temperature,
Carrier gas flux is 10ml/min.
3, reagent
Methanol, chromatographically pure
The dilution process of methanol Standard Gases: distribution is diluted (with reference to " empty with 100ml all-glass syringe as needed
Gas and waste gas monitoring analysis method " (1990) P42).
4, sample acquires:
4.1 organized emission monitoring samplings
4.1.1 sampling location and sampled point
Sampling location and sampled point are determined by 9.1.1 in GB16157-1996 and 9.1.2.
4.1.2 the connection of sampling apparatus
With reference to 9.3 Figure 30 in GB16157-1996, by the suitable of sampling pipe, sampler, flow measurement device and aspiration pump
Sequence connects sampling system, and by GB16157-1996 9.4 requirement, checks the air-tightness and reliability of sampling system "
4.1.3 sample acquires
In the sampling appropriate mineral wool of tube head plug, and exhaust tube sampled point is protruded into, starts aspiration pump, it first will sampling
System pipeline is sufficiently cleaned with the gas in exhaust tube, then twitches syringe, after washing 5-6 times repeatedly, pumps full required volume
Gas.It is sealed with rubber cap (inner liner polytetrafluoroethylene film) rapidly, takes back laboratory.
4.2 uncontrollable discharge monitoring sampling
4.2.1 sampling location and sampled point
The position of uncontrollable discharge monitoring point is determined by the regulation of appendix C in GB16297-1996, or specific is wanted by other
Seek determining sampling environment air point.
4.2.2 sample acquires
At sampled point scene, after first washing sampling syringe 5-6 times repeatedly, live air, rapid sealing injection are pumped full
Device mouth, takes back lab analysis.If necessary, sample gas can be repeatedly washed with syringe, after being injected into bladder tank, takes back reality
Test room.
4.2.3 blank sample is sampled as bringing syringe to sampled point, in addition to being not connected to samplers sample air sample,
The remaining same sample of operation.
4.2.4 sample saves
It should be analyzed as early as possible after sample.Cannot such as analyze in time, can the 3-5 DEG C of refrigeration in refrigerator, analysis in a week
It finishes.
5, analysis measurement:
5.1 sample handling procedures are that the sample being stored in aluminium foil bag or 100ml syringe is taken with 1ml syringe
Gas takes 1.0ml sample gas to be analyzed after replacing 3 times repeatedly.If concentration is more than measurement range, cleaned air or height can be used
It is measured after pure nitrogen gas dilution, multiplied by extension rate when calculating.
The preparation and measurement of 5.2 standard gas: it prepares: taking 1ul methanol (fine chemistry industry research institute is recovered in colour code, Tianjin), add
Enter to be placed in 100ml syringe to dry in 40 DEG C of baking ovens and be made into standard gas 1 for a moment, then takes 10ml to be diluted to 100ml in standard gas 1,
It is made into 7.918*10-4The dense mark standard gas of mg/ml, then respectively draw 0,2,5,10, the dense standard gas body of 20ml into 100ml syringe, according to
It is secondary to be made into 0,15.8ug/l, 39.6ug/l, 79.2ug/l, 158.4ug/l standard series, it measures under prescribed conditions.
The production of 5.3 standard curves: conditioning instrumentation operating condition, sample introduction 1.0ml measure each standard series, each concentration
Replication 3 times, standard curve is drawn to corresponding methanol concentration with peak height or peak area mean value.
5.4 measurements: one, the similarity condition for measuring standard series measures blank control, obtains peak height or peak area value；Two,
Measure standard series similarity condition measure sample gas, the sample peak height or peak area value measured subtract blank control peak height or
After peak area value, the concentration of methanol in sample is obtained by standard curve.
6, sample concentration calculation method:
Calculate the concentration of methanol in air
CSample=K* (YSample-a)/b
In formula: CSample--- to the methanol concentration in test sample, mg/m3
YSample--- to the methanol peak height (or peak area) in test sample, mm
The extension rate of K --- sample to be tested
A, b --- it is respectively the intercept and slope of equation of linear regression
Embodiment 2
Precision test experiments of the invention:
The above-mentioned 7.918*10 of 5.0ml is drawn respectively-4In four parts to four 100mL syringes of calibrating gas of ug/ml, respectively
Label 1,2,3 and 4 carries out the measurement of sample concentration by the sample measuring method of embodiment 1, as a result as follows:
It is computed, the mean concentration of methanol is 40.4 μ g/l, and coupon results show that the Precision Experiment of methanol complies with standard
Defined requirement.
Embodiment 3
Recovery of standard addition experiment: drawing 10.0ml methanol concentration respectively is 7.918*10-4Ug/l calibrating gas is to embodiment 2
100ml syringe in, respective recovery of standard addition is as shown in the table:
By calculating:
1 recovery of standard addition of sample: 92.9%；2 recovery of standard addition of sample: 94.8%；
3 recovery of standard addition of sample: 93.7%；4 recovery of standard addition of sample: 93.3%.
The measurement of methanol is analyzed in existing national standard method with packed column in the exhaust of solid pollution source.According to standard
It is required that disparity items requires to use different chromatographic columns, and the packed column utilization rate required in standard is lower, in addition to measuring methanol
Outer few other projects use the chromatographic column, and a root chromatogram column price is expensive (one, the more members of packed column about 1000-2000),
A root chromatogram column is bought, and utilization rate is not high, so feeling to waste very much.So to select the suitable and higher chromatography of utilization rate
Column and suitable column temperature, temperature of vaporization chamber, detection room temperature and carrier gas flux.PEG-20M capillary is selected, PEG-20M is one
The kind very high capillary column of utilization rate, many detection projects all use the chromatographic column, after setting suitable determination condition, simultaneously also
The detection that can carry out other compounds solves the problems, such as to be replaced as frequently as pillar and easily causes the damage of pillar and time-consuming, both
Save the time saving accuracy that more importantly ensure that data again.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (5)
1. the measuring method of methanol in a kind of solid pollution source exhaust, characterized by the following steps:
(1) sample acquires: including sampling in a organized way, inorganization sampling and blank sample sampling；The inorganization sampling is sampling
Point scene, after first washing sampling syringe 5-6 times repeatedly, pumps full live air, rapid sealing injection device mouth takes back laboratory
Analysis；Organized sampling is protruded into exhaust tube sampled point in the sampling appropriate mineral wool of tube head plug, starts aspiration pump, first
Sampling system pipeline is sufficiently cleaned with the gas in exhaust tube first, then twitches syringe, after washing 5-6 times repeatedly, is pumped full
The gas of required volume, and sealed with rubber cap rapidly, take back laboratory；The blank sample is sampled as bringing syringe to adopting
Sampling point, in addition to being not connected to samplers sample air sample, remaining operates same sample；
(2) sample treatment: taking the sample gas being stored in aluminium foil bag or 100ml syringe with 1ml syringe, replaces 3 times repeatedly
Afterwards, it takes 1.0ml sample gas to be analyzed, if concentration is more than measurement range, is surveyed after being diluted with cleaned air or high pure nitrogen
Calmly, multiplied by extension rate when calculating；
(3) preparation of calibrating gas: being diluted distribution with 100ml all-glass syringe as needed, takes methanol Standard Gases, root
According to the concentration of sample to be tested, in the range of linearity 5.0-1.0*10 of methanol4mg/m3Interior cleaned air or high pure nitrogen dilution are matched
It is set to the standard series of 15.8ug/l, 39.6ug/l, 79.2ug/l, 158.4ug/l concentration；
(4) production and measurement of standard curve: gas chromatograph is adjusted to optimum determining state, sample introduction 1.0ml measures each mark
Quasi- series, each concentration replication 3 times, the peak height for measuring each concentration of standard series respectively or peak area mean value are to corresponding first
Alcohol standard gas concentration draws standard curve or calculates regression equation.
2. the measuring method of methanol in a kind of solid pollution source exhaust according to claim 1, it is characterised in that: step
(1) in inorganization sampling if necessary, sample gas can be repeatedly washed with syringe, after being injected into bladder tank, takes back laboratory.
3. the measuring method of methanol in a kind of solid pollution source exhaust according to claim 1, it is characterised in that: step
(1) rubber cap is lined with polytetrafluoroethylene film in.
4. the measuring method of methanol in a kind of solid pollution source exhaust according to claim 1, it is characterised in that: step
(4) gas phase condition of gas chromatograph is set as using PEG-20M capillary chromatographic column 30m*0.50mm* in determination step
1.0um, column temperature are 70 degree, and temperature of vaporization chamber is 200 degree, and detection room temperature is 230 degree, carrier gas flux 10ml/min.
5. the measuring method of methanol in a kind of solid pollution source exhaust according to claim 1, it is characterised in that: step
(4) measurement includes sample measurement and reference substance measurement, and the reference substance is measured as measurement blank control cleaned air, obtains peak height
Or peak area value；The sample is measured as the similarity condition measurement sample gas with measurement standard series, the sample peak height measured
Or after peak area value subtracts blank control peak height or peak area value, the concentration of methanol in sample is obtained by standard curve.
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Cited By (2)
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| CN110887908A (en) * | 2019-12-05 | 2020-03-17 | 中维安全检测认证集团有限公司 | Method for detecting ethylene in gas by gas chromatography |
| CN112666276A (en) * | 2020-11-30 | 2021-04-16 | 浙江必利夫检测科技有限公司 | Gas chromatograph for detecting alcohols and detection method thereof |
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| CN110887908A (en) * | 2019-12-05 | 2020-03-17 | 中维安全检测认证集团有限公司 | Method for detecting ethylene in gas by gas chromatography |
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| CN112666276A (en) * | 2020-11-30 | 2021-04-16 | 浙江必利夫检测科技有限公司 | Gas chromatograph for detecting alcohols and detection method thereof |
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