CN110487926A - The measuring method of acrylonitrile in a kind of Concentration in Fixed Pollutants Source - Google Patents
The measuring method of acrylonitrile in a kind of Concentration in Fixed Pollutants Source Download PDFInfo
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- CN110487926A CN110487926A CN201910731974.XA CN201910731974A CN110487926A CN 110487926 A CN110487926 A CN 110487926A CN 201910731974 A CN201910731974 A CN 201910731974A CN 110487926 A CN110487926 A CN 110487926A
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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 a kind of measuring methods of acrylonitrile in Concentration in Fixed Pollutants Source, it include: sample acquisition, sample treatment, the preparation of standard solution and measurement, the production of standard curve and the several steps of measurement, wherein sample acquisition includes short time sampling, for a long time sampling and blank sample sampling；Sample treatment is to pour into front and back section active carbon in two solvent desorption bottles respectively, each that 1.0mL carbon disulfide is added, and after closing, desorbs 30min, shakes frequently.Sample solution is for measurement；The gas phase condition of gas chromatograph is set as using 30m × 0.32mm × 0.5 μm, FFAP capillary chromatographic column in determination step, and column temperature is 70 DEG C, keeps 6min；Temperature of vaporization chamber is 200 DEG C, and detection room temperature is 250 DEG C, carrier gas flux 1.5mL/min；Split ratio: 20: 1.After method of the invention sets suitable determination condition, the detection of other compounds in nitrile compounds can also be carried out simultaneously, it solves the problems, such as to be replaced as frequently as pillar and easily causes the damage of pillar and time-consuming, not only saved but also the time saving accuracy that more importantly ensure that data.
Description
Technical field
The present invention relates to a kind of measuring methods of acrylonitrile in Concentration in Fixed Pollutants Source, belong to compound chemical detection neck
Domain.
Background technique
Gas chromatography, national standard HJ/ are usually used for the measuring method of acrylonitrile in Concentration in Fixed Pollutants Source
The determination condition of acrylonitrile is 3m × 3mmGDX-502,60~80 mesh glass columns, column temperature: 130 DEG C in T37-1999；Vaporization
Room temperature: 150 DEG C；Detection room temperature: 150 DEG C；Carrier gas (nitrogen) flow: 30mL/min.Likewise, toxic for other class air
Gas chromatography can also be used in the measurement of substance, 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 5000 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 suitable capillary column, is applicable in the measurement of each substance, same compound is each
The condition of kind of project measurement, and ensure that every detection data is accurate and meets the requirements, it is accurate to accomplish to save time saving and data
Multiple advantage, be researcher's urgent need to solve the problem in current detection industry.
Summary of the invention
Goal of the invention: the present invention aiming at the shortcomings in the prior art, provides acrylonitrile in a kind of Concentration in Fixed Pollutants Source
There is measuring method cost to reduce, and save time, the high advantage of accuracy.
Technical solution: the measuring method of acrylonitrile in a kind of Concentration in Fixed Pollutants Source of the present invention, including walk as follows
It is rapid:
(1) sample acquires: including short time sampling, for a long time sampling and blank sample sampling；Short time is sampled as adopting
Sampling point opens activated carbon tube both ends, with 100mL/min flow collection 15min air sample；It is sampled as a long time in sampled point,
Activated carbon tube both ends are opened, with 50mL/min flow collection 2~8h air sample, closing activity charcoal pipe both ends at once after sampling,
Transport in cleaning container is set to save；Blank sample is sampled as bringing activated carbon tube to sampled point, is opened both ends and is closed immediately, so
It transports, save and measures together with sample afterwards；
(2) sample treatment: front and back section active carbon is poured into respectively in two solvent desorption bottles, each that 1.0mL curing is added
Carbon after closing, desorbs 30min, shakes frequently.Sample solution is for measurement；
(3) preparation and measurement of standard solution: being added carbon disulfide in volumetric flask, after precise, is separately added into certain
The acrylonitrile of amount, then precise；Then plus carbon disulfide is to scale, and the concentration of solution is calculated by the difference weighed, is acrylonitrile
Standard solution；
(4) production and measurement of standard curve: taking 5 volumetric flasks, with carbon disulfide working solution at 40.5 μ g/
ML, 81 μ g/mL, 162 μ g/mL, 243 μ g/mL, 324 μ g/mL concentration ranges acrylonitrile standard series, referring to instrumentation item
Gas chromatograph is adjusted to optimum determining state by part, and 1.0 μ L of sample introduction measures the peak height or peak of each concentration of standard series respectively
Area draws standard curve with the corresponding acrylonitrile concentration of peak height or peak area (μ g/mL) measured or calculates regression equation,
Related coefficient answers >=0.999.
Further, in step (4) determination step the gas phase condition of gas chromatograph be set as using 30m × 0.32mm ×
0.5 μm, FFAP capillary chromatographic column, column temperature is 70 DEG C, keeps 6min；Temperature of vaporization chamber is 200 DEG C, and detection room temperature is 250
DEG C, carrier gas flux 1.5mL/min；Split ratio: 20: 1.
Further, with the operating condition measurement sample solution and sample of measurement standard series in step (4) determination step
Blank solution, the peak height or peak area value measured are obtained the concentration μ g/ of acrylonitrile in sample solution by standard curve or regression equation
ML is measured after being diluted with carbon disulfide if testing concentration is more than measurement range in sample solution, multiplied by dilution times when calculating
Number.
The utility model has the advantages that in this Concentration in Fixed Pollutants Source of the invention acrylonitrile measuring method, using 30m × 0.32mm
× 0.5 μm, FFAP capillary chromatographic column, column temperature is 70 DEG C, keeps 6min；Temperature of vaporization chamber is 200 DEG C, and detection room temperature is
250 DEG C, carrier gas flux 1.5mL/min；Split ratio: 20: 1.Detect the result testing number of acrylonitrile in Concentration in Fixed Pollutants Source
According to accurate, meet national requirements, time-saving and efficiency.
30m × 0.32mm × 0.5 μm is selected, FFAP capillary chromatographic column after setting suitable determination condition, while may be used also
To carry out the detection of other compounds in nitrile compounds, solves and be replaced as frequently as pillar and easily cause the damage of pillar and time-consuming
The problem of, it had not only saved but also the time saving accuracy that more importantly ensure that data.
Specific embodiment
The present invention is further explained in the light of specific embodiments:
Embodiment 1
The measuring method of acrylonitrile in a kind of Concentration in Fixed Pollutants Source, including sample acquisition, sample treatment, standard solution
It prepares and measures, the production and measurement of standard curve, specifically comprise the following steps:
Sample acquisition: the short time is sampled as activated carbon tube both ends being opened, with 100mL/min flow collection in sampled point
15min air sample；It is sampled as opening activated carbon tube both ends in sampled point for a long time, it is empty with 2~8h of 50mL/min flow collection
Gas sample product；Closing activity charcoal pipe both ends at once after sampling are set transport in cleaning container and are saved.Blank sample is sampled as active carbon
Pipe is brought to sampled point, is opened both ends and is closed immediately, is then transported, saves and is measured together with sample.Sample at room temperature may be used
It saves 5 days.
Sample treatment: front and back section active carbon is poured into respectively in two solvent desorption bottles, each that 1.0mL carbon disulfide is added,
After closing, 30min is desorbed, is shaken frequently.Sample solution is for measurement.
Standard solution: being added carbon disulfide in volumetric flask, after precise, is separately added into a certain amount of acrylonitrile, then quasi-
Really weigh；Then plus carbon disulfide is to scale, and the concentration of solution is calculated by the difference weighed, is acrylonitrile standard solution.Or use state
The standard solution that family is approved is prepared.
The preparation of standard curve: taking 5 volumetric flasks, with carbon disulfide working solution at 40.5 μ g/mL, 81 μ g/mL,
162 μ g/mL, 243 μ g/mL, 324 μ g/mL concentration ranges acrylonitrile standard series.Referring to instrumentation condition, by gas phase color
Spectrometer is adjusted to optimum determining state, and 1.0 μ L of sample introduction measures the peak height or peak area of each concentration of standard series respectively.To measure
Peak height or the corresponding acrylonitrile concentration of peak area (μ g/mL) draw standard curve or calculate regression equation, related coefficient answers
≥0.999。
Sample measurement: with the operating condition measurement sample solution and sample blank solution of measurement standard series, the peak measured
High or peak area value is obtained the concentration (μ g/mL) of acrylonitrile in sample solution by standard curve or regression equation.If in sample solution
Testing concentration is more than measurement range, is measured after being diluted with carbon disulfide, multiplied by extension rate when calculating.Gas phase in determination step
Chromatographic gas phase condition is set as using 30m × 0.32mm × 0.5 μm, FFAP capillary chromatographic column, and column temperature is 70 DEG C, is kept
6min；Temperature of vaporization chamber is 200 DEG C, and detection room temperature is 250 DEG C, carrier gas flux 1.5mL/min；Split ratio: 20: 1.
The measuring method of acrylonitrile in this Concentration in Fixed Pollutants Source of the invention, using 30m × 0.32mm × 0.5 μm,
FFAP capillary chromatographic column, column temperature are 70 DEG C, keep 6min；Temperature of vaporization chamber is 200 DEG C, and detection room temperature is 250 DEG C, carrier gas
Flow is 1.5mL/min；Split ratio: 20: 1.The result detection data for detecting acrylonitrile in Concentration in Fixed Pollutants Source is accurate, meets
National requirements, time-saving and efficiency.
30m × 0.32mm × 0.5 μm is selected, FFAP capillary chromatographic column after setting suitable determination condition, while may be used also
To carry out the detection of other compounds in nitrile compounds, solves and be replaced as frequently as pillar and easily cause the damage of pillar and time-consuming
The problem of, it had not only saved but also the time saving accuracy that more importantly ensure that data.
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 (3)
1. the measuring method of acrylonitrile in a kind of Concentration in Fixed Pollutants Source, characterized by the following steps:
(1) sample acquires: including short time sampling, for a long time sampling and blank sample sampling；Short time is sampled as in sampled point,
Activated carbon tube both ends are opened, with 100mL/min flow collection 15min air sample；It is sampled as opening and living in sampled point for a long time
Property charcoal pipe both ends, with 50mL/min flow collection 2~8h air sample, cleaning is set at closing activity charcoal pipe both ends at once after sampling
Transport saves in container；Blank sample is sampled as bringing activated carbon tube to sampled point, is opened both ends and is simultaneously closed immediately, then with sample
Product are transported together, save and are measured；
(2) sample treatment: front and back section active carbon is poured into respectively in two solvent desorption bottles, each that 1.0mL carbon disulfide, envelope is added
After closing, 30min is desorbed, is shaken frequently.Sample solution is for measurement；
(3) preparation and measurement of standard solution: being added carbon disulfide in volumetric flask, after precise, is separately added into a certain amount of
Acrylonitrile, then precise；Then plus carbon disulfide is to scale, and the concentration of solution is calculated by the difference weighed, is acrylonitrile standard
Solution；
(4) production and measurement of standard curve: taking 5 volumetric flasks, with carbon disulfide working solution at 40.5 μ g/mL, 81 μ
G/mL, 162 μ g/mL, 243 μ g/mL, 324 μ g/mL concentration ranges acrylonitrile standard series, referring to instrumentation condition, by gas
Chromatography is adjusted to optimum determining state, and 1.0 μ L of sample introduction measures the peak height or peak area of each concentration of standard series respectively, with
The corresponding acrylonitrile concentration of peak height or peak area (μ g/mL) measured draws standard curve or calculates regression equation, phase relation
Number answers >=0.999.
2. the measuring method of acrylonitrile in a kind of Concentration in Fixed Pollutants Source according to claim 1, it is characterised in that: step
(4) gas phase condition of gas chromatograph is set as using 30m × 0.32mm × 0.5 μm, FFAP capillary chromatography in determination step
Column, column temperature are 70 DEG C, keep 6min；Temperature of vaporization chamber is 200 DEG C, and detection room temperature is 250 DEG C, carrier gas flux 1.5mL/
min；Split ratio: 20: 1.
3. the measuring method of acrylonitrile in a kind of Concentration in Fixed Pollutants Source according to claim 1, it is characterised in that: step
(4) with the operating condition measurement sample solution and sample blank solution of measurement standard series in determination step, the peak height measured or
Peak area value is obtained the concentration μ g/mL of acrylonitrile in sample solution by standard curve or regression equation, if determinand in sample solution
Concentration is more than measurement range, is measured after being diluted with carbon disulfide, multiplied by extension rate when calculating.
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| US20070289360A1 (en) * | 2004-08-14 | 2007-12-20 | Michael Horstmann | Monitoring System For Collecting And/Or Transdermally Rediffusing Air Containing Environmental Contaminants, And Corresponding Method |
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| CN110045033A (en) * | 2019-04-28 | 2019-07-23 | 浙江鑫泰检测技术有限公司 | A kind of method of benzene homologues in detection workplace air |
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