CN105181851A - Method for testing oxynitride in environment - Google Patents
Method for testing oxynitride in environment Download PDFInfo
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- CN105181851A CN105181851A CN201510657748.3A CN201510657748A CN105181851A CN 105181851 A CN105181851 A CN 105181851A CN 201510657748 A CN201510657748 A CN 201510657748A CN 105181851 A CN105181851 A CN 105181851A
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Abstract
The invention provides a method for testing oxynitride in the environment. The test method comprises the following steps: nitric oxides in a standard sample are sent to a chromatographic test column by a discharge ionization detector and through steps of isolation and cutting reverse blowing, and standard chromatograms of all the nitric oxides in the standard sample are obtained; peak areas of all the nitric oxides in the standard sample are obtained according to the standard chromatograms, and correction factors of all the nitric oxides are calculated according to the peak areas of all the nitric oxides in the standard sample and the concentration of all the nitric oxides in the standard sample; to-be-tested gas is tested with gas chromatography test conditions which are same with the standard sample, test chromatograms of nitric oxides in to-be-tested air are obtained, and the concentration of each nitric oxide which is equal to the correction factor multiplying the peak area of the corresponding nitric oxide in the to-be-tested gas is calculated according to the peak areas of all the nitric oxides in the test chromatograms. The test method has the advantages that the sampling process is simple and rapid, the accuracy and the sensitivity are high, the detection limit is low and the like.
Description
Technical field
The present invention relates to chemical analysis chemical examination field, the assay method of oxides of nitrogen in a kind of environment.
Background technology
Along with the fast development of suitability for industrialized production, the existence of oxynitrides has serious harmfulness to environment, the mankind, exerts a certain influence to safety in production simultaneously.Such as, divide in air compressing device at sky, when nitrogen monoxide is by air compressor, can be polymerized or selective oxidation, and then being suspended in liquid air surface after causing organic hydrocarbon compounds to be separated out with solid in the liquid air of deep cooling, the shock fierce on rapid liquid air surface, frictional sparking can produce explosion danger.The oxynitride concentration of separate sources is different, carries out analyzing measuring the means adopted and being also not quite similar it.At present, in mensurated gas composition, the method for oxynitrides mainly contains: the methods such as vapor-phase chromatography, chemoluminescence method, infra-red sepectrometry, solution absorption method, solid sorbent method.
But said method exists shortcomings, such as complex operation, cost are high, with duration, accuracy is low, detector sensitivity is lower, can not meet the requirement that modern enterprise is produced fast.Therefore, how to set up a kind of method of novel, quick, Accurate Determining oxynitrides, measure requirement to adapt to environmental protection air monitering, air separation unit liquid nitrogen product and nitrogen oxides of exhaust gas, become the technical barrier that this area is urgently to be resolved hurrily.
Summary of the invention
Fundamental purpose of the present invention is the assay method providing oxides of nitrogen in a kind of environment, with set up a kind of fast, the method for Accurate Determining oxynitrides.
To achieve these goals, the invention provides the assay method of oxides of nitrogen in a kind of environment, this assay method comprises the following steps: utilize chromatography with discharge ionization detector and enter chromatogram test pole by the oxides of nitrogen in standard model and carry out by isolation, cutting blowback step, the standard colors spectrogram of each oxides of nitrogen in getting standard samples; The peak area of each oxides of nitrogen in getting standard samples according to standard colors spectrogram, and the concentration of each oxides of nitrogen in the peak area of each oxides of nitrogen and standard model according to standard sample, calculate the correction factor of each oxides of nitrogen; The gas chromatography test condition identical with standard model is utilized to test gas to be measured, obtain the test color spectrogram of each oxides of nitrogen in air to be measured, and the peak area of each oxides of nitrogen in the spectrogram of side is tested according to this, calculate the peak area of corresponding oxides of nitrogen in the concentration=correction factor × gas to be measured of each oxides of nitrogen in testing sample.
Further, standard model is made up of multiple calibrating gas, and each calibrating gas is by NO, N
2o and He forms.
Further, in each calibrating gas, the concentration of NO is 0.1 ~ 10ppm, N
2the concentration of O is 0.1 ~ 10ppm.
Further, the step of standard colors spectrogram of each oxides of nitrogen of getting standard samples comprises: be injected in gas chromatograph respectively according to nitrous oxides concentration order from low to high by each calibrating gas, and utilizes chromatography with discharge ionization detector in gas chromatograph to carry out detection to obtain standard colors spectrogram.
Further, in getting standard samples, the step of the concentration of each oxides of nitrogen comprises: utilize gas chromatograph to standard model replication n time, the concentration measurement of each oxides of nitrogen in getting standard samples, n >=2; N concentration measurement of oxides of nitrogen each in standard model is averaged, and using the concentration of mean value corresponding oxides of nitrogen in standard model.
Further, standard model is made up of with the volume ratio of 1:1 the first calibrating gas and the second calibrating gas; In first calibrating gas, the concentration of NO is 5ppm, N
2the concentration of O is 5ppm; In second calibrating gas, the concentration of NO is 1ppm, N
2the concentration of O is 1ppm; 2≤n>=5.
Further, in the correction factor=standard model of each oxides of nitrogen each oxides of nitrogen concentration/standard model in the peak area of corresponding oxides of nitrogen.
Further, gas to be measured comprises hydrogen, oxygen and carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon; Test to gas to be measured the step obtaining test color spectrogram to comprise: gas to be measured is passed in the pre-column of gas chromatograph, component separation is carried out after utilizing heartcut principle to make gas to be measured enter pre-column, and peak sequence is hydrogen, oxygen and carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon, after oxides of nitrogen enters separating column from pre-column outflow, by other component from atmospheric valve emptying; Utilize that the separating column in gas chromatograph and chromatography with discharge ionization detector are separated, the oxides of nitrogen detected in gas to be measured, and obtain test color spectrogram.
Further, the step that the step that obtains test color spectrogram comprises is tested to gas to be measured and comprises: step S1, open sample introduction valve, make each component in gas to be measured flow into pre-column, make each component carry out pre-separation; Each oxides of nitrogen in step S2, gas to be measured flows out from pre-column, and transfer valve after inflow separating column, makes other impurity composition blowback emptying; Be separated successively with the method for step S2 according to step S1, each oxides of nitrogen detected in gas to be measured, obtain the test color spectrogram of each oxides of nitrogen.
Further, the sensitivity of gas chromatograph is less than 10mg/m
3.
Apply technical scheme of the present invention, assay method provided by the invention only need prepare the correction factor that Standard Gases is demarcated, can calculate the peak area of corresponding oxides of nitrogen in the concentration=correction factor × gas to be measured of each oxides of nitrogen in testing sample, and this assay method has, and sampling process is simple, quick, accurate determines the advantages such as high, detection limit is low.The additive methods such as this assay method chromatography only needs 10 minutes just can go out result, this time colourimetry are incomparable.
Accompanying drawing explanation
The Figure of description forming a application's part is used to provide a further understanding of the present invention, and schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows the schematic diagram of the assay method of oxides of nitrogen in the environment provided according to embodiments of the invention.
Embodiment
It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.Below with reference to the accompanying drawings and describe the application in detail in conjunction with the embodiments.
It should be noted that used term is only to describe embodiment here, and be not intended to the illustrative embodiments of restricted root according to the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative is also intended to comprise plural form, in addition, it is to be further understood that, " comprise " when using term in this manual and/or " comprising " time, it indicates existing characteristics, step, operation, device, assembly and/or their combination.
From background technology, in existing border there is shortcomings in the assay method of oxides of nitrogen, and such as complex operation, cost are high, with duration, accuracy is low, detector sensitivity is lower, can not meet the requirement that modern enterprise is produced fast.The present inventor studies for the problems referred to above, proposes the assay method of oxides of nitrogen in a kind of environment.As shown in Figure 1, this assay method comprises the following steps: utilize chromatography with discharge ionization detector and by isolation, cut the step such as blowback and allow the oxides of nitrogen in standard model enter chromatogram test pole to carry out, the standard colors spectrogram of each oxides of nitrogen in getting standard samples; The peak area of each oxides of nitrogen in getting standard samples according to standard colors spectrogram, and the concentration of each oxides of nitrogen in the peak area of each oxides of nitrogen and standard model according to standard sample, calculate the correction factor of each oxides of nitrogen; The gas chromatography test condition identical with standard model is utilized to test gas to be measured, obtain the test color spectrogram of each oxides of nitrogen in air to be measured, and the peak area of each oxides of nitrogen in the spectrogram of side is tested according to this, calculate the peak area of corresponding oxides of nitrogen in the concentration=correction factor × gas to be measured of each oxides of nitrogen in testing sample.
Assay method provided by the invention only need prepare the correction factor that Standard Gases is demarcated, can calculate the peak area of corresponding oxides of nitrogen in the concentration=correction factor × gas to be measured of each oxides of nitrogen in testing sample, and this assay method has, and sampling process is simple, quick, accurate determines the advantages such as high, detection limit is low.The additive methods such as this assay method chromatography only needs 10 minutes just can go out result, this time colourimetry are incomparable.
In assay method provided by the invention, gas chromatograph can adopt advanced in years company of the U.S., and this gas chromatograph is configured with helium chromatography with discharge ionization detector (DID).The helium adopted in standard model is preferably high-purity helium (purity is 99.99999%).The volume of stainless steel sampling steel cylinder can be 1000ml, inner inerting disposal.
In above-mentioned helium chromatography with discharge ionization detector (DID), the sparking electrode in arc chamber imposes suitable voltage and produce electric discharge, obtain a branch of high energy UV; He in high-purity helium is excited to metastable state He* by electrode discharge; Metastable state He* is introduced into ionization chamber by slit, and by component ionization each in sample gas, ion is ionized indoor polarized electrode and collects, and is namely composed peak accordingly through amplifying.DID detector applies, in the trace impurity analysis of high-purity gas, has very high sensitivity.In order to ensure the accuracy that whole subsystem detects and low detection limit, whole system material all selects interior polishing pipeline and the VCR pipe fitting joint without dead volume, and ensure that the accuracy of high-purity gas trace analysis, its sensitivity is less than 10mg/m
3.
The detection limit computing method of application gas chromatograph are: minimum detectability=3 × noise × concentration/peak height, after baseline is steady, is 0.0466, calculates N from spectrogram readout noise
2o minimum detectability 0.010mg/L, NO minimum detectability 0.004mg/L.
Illustrative embodiments according to the assay method of oxides of nitrogen in environment provided by the invention will be described in more detail below.But these illustrative embodiments can be implemented by multiple different form, and should not be interpreted as being only limited to embodiment set forth herein.Should be understood that, provide these embodiments be in order to make the application open thorough and complete, and the design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
First, utilize chromatography with discharge ionization detector and by isolation, cut the step such as blowback and allow the oxides of nitrogen in standard model enter chromatogram test pole to carry out, the standard colors spectrogram of each oxides of nitrogen in getting standard samples.
Wherein, standard model is made up of multiple calibrating gas, and each calibrating gas is preferably by NO, N
2o and He forms.Preferably, in each calibrating gas, the concentration of NO is 0.1 ~ 10ppm, N
2the concentration of O is 0.1 ~ 10ppm.Preferably, standard model is made up of with the volume ratio of 1:1 the first calibrating gas and the second calibrating gas; In first calibrating gas, the concentration of NO is 5ppm, N
2the concentration of O is 5ppm; In second calibrating gas, the concentration of NO is 1ppm, N
2the concentration of O is 1ppm; 2≤n>=5.More preferably, standard model is made up of 4 calibrating gas, and its concentration asks for an interview table 1.It should be noted that the standard 1 in table 1, standard 2, standard 3 and standard 4 represent a calibrating gas respectively.
Table 1
Above-mentioned get standard samples in the step of standard colors spectrogram of each oxides of nitrogen can comprise: each calibrating gas (standard 1, standard 2, standard 3 and standard 4) is injected in gas chromatograph respectively according to nitrous oxides concentration order from low to high, and utilizes chromatography with discharge ionization detector in gas chromatograph to carry out detection to obtain standard colors spectrogram.
In this step, chromatographic column condition is as shown in table 2 below.
Table 2
Then, the peak area of each oxides of nitrogen in getting standard samples according to standard colors spectrogram, and the concentration of each oxides of nitrogen in the peak area of each oxides of nitrogen and standard model according to standard sample, calculate the correction factor of each oxides of nitrogen.
Above-mentioned get standard samples in the step of concentration of each oxides of nitrogen can comprise: utilize gas chromatograph to standard model replication n time, the concentration measurement of each oxides of nitrogen in getting standard samples, n >=2; N concentration measurement of oxides of nitrogen each in standard model is averaged, and using the concentration of mean value corresponding oxides of nitrogen in standard model.
Particularly, calibrating gas 2 and calibrating gas 3 are mixed as testing sample using the ratio of 1:1, replication 5 times under above-mentioned chromatographic condition, measurement result is as shown in table 3.
Table 3
Particularly, in the correction factor=described standard model of each described oxides of nitrogen each oxides of nitrogen concentration/described standard model in the peak area of corresponding oxides of nitrogen.
Finally, the gas chromatography test condition (test condition that with table 1 provide identical) identical with described standard model is utilized to test gas to be measured, obtain the test color spectrogram of each oxides of nitrogen in described air to be measured, and the peak area of each oxides of nitrogen in the spectrogram of side is tested according to this, calculate the peak area of corresponding oxides of nitrogen in the concentration=described correction factor × described gas to be measured of each oxides of nitrogen in testing sample
In this step, preferably, gas to be measured comprises hydrogen, oxygen and carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon; Test to gas to be measured the step obtaining test color spectrogram to comprise: gas to be measured is passed in the pre-column of gas chromatograph; Control the switch of the valve of column oven in gas chromatograph, make the hydrogen in gas to be measured, air and carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon flow out pre-column successively and enter column oven; Chromatography with discharge ionization detector in gas chromatograph is utilized to detect the test color spectrogram of hydrogen, oxygen and carbon monoxide in gas to be measured, methane, carbon dioxide, oxides of nitrogen and hydrocarbon successively.
More specifically, test to gas to be measured the step that the step that obtains test color spectrogram comprises to comprise: step S1, open the valve of column oven, make the hydrogen in gas to be measured flow out pre-column and enter the test color spectrogram that chromatography with discharge ionization detector carries out detecting the hydrogen obtained in gas to be measured; Step S2, flow out the valve of closing column oven after pre-column until the hydrogen in gas to be measured; The test color spectrogram of air in gas to be measured and carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon is detected successively according to the method for step S1 and step S2.Preferably, each time of closing the valve of column oven is 10s ~ 10min.
Concrete test process is: open gas chromatograph and adjust flow rate of carrier gas, analytical approach is set up according to chromatographic condition, when baseline stability, analyze during calibrating gas is injected into on-line dilution system high-accuracy chromatograph via carburetor and ten logical sampling valves respectively according to concentration order from low to high, detect with DID detecting device and obtain standard colors spectrogram.Determine retention time and the peak area of each component, with each concentration of component for horizontal ordinate, peak area is ordinate, and drawing standard curve carries out linear regression, and determines regression equation.Incision principle centered by its measuring mechanism, namely after sample enters pre-column (precolumn), carries out component separation through pre-column, peak sequence is followed successively by hydrogen, oxygen adds carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon.As NO and N
2o flows out from pre-column, enter column oven (column), and hydrocarbon finally flows out.Wherein, the actuation time of valve is as shown in table 2 below.(wherein, valve 2 and valve 4 are control to carry out after gas to be measured enters pre-column the valve that component is separated in gas chromatograph).
Table 2
As can be seen from the above embodiments, the above-mentioned example of the present invention achieves following technique effect: assay method provided by the invention only need prepare the correction factor that Standard Gases is demarcated, can calculate the peak area of corresponding oxides of nitrogen in the concentration=correction factor × gas to be measured of each oxides of nitrogen in testing sample, and this assay method has, and sampling process is simple, quick, accurate determines the advantages such as high, detection limit is low.The additive methods such as this assay method chromatography only needs 10 minutes just can go out result, this time colourimetry are incomparable.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the assay method of oxides of nitrogen in environment, it is characterized in that, described assay method comprises the following steps:
Utilize chromatography with discharge ionization detector and enter chromatogram test pole by the oxides of nitrogen in standard model carry out by isolation, cutting blowback step, obtaining the standard colors spectrogram of each described oxides of nitrogen in described standard model;
The peak area of each described oxides of nitrogen in getting standard samples according to standard colors spectrogram, and according to the concentration of each described oxides of nitrogen in the peak area of described oxides of nitrogen each in described standard model and described standard model, calculate the correction factor of each described oxides of nitrogen;
The gas chromatography test condition identical with described standard model is utilized to test gas to be measured, obtain the test color spectrogram of each oxides of nitrogen in described air to be measured, and the peak area of each oxides of nitrogen in the spectrogram of side is tested according to this, calculate the peak area of corresponding oxides of nitrogen in the concentration=described correction factor × described gas to be measured of each oxides of nitrogen in testing sample.
2. assay method according to claim 1, is characterized in that, described standard model is made up of multiple calibrating gas, and each described calibrating gas is by NO, N
2o and He forms.
3. assay method according to claim 2, is characterized in that, in each described calibrating gas, the concentration of described NO is 0.1 ~ 10ppm, described N
2the concentration of O is 0.1 ~ 10ppm.
4. assay method according to any one of claim 1 to 3, it is characterized in that, the step obtaining the standard colors spectrogram of each described oxides of nitrogen in described standard model comprises: be injected into respectively in described gas chromatograph according to nitrous oxides concentration order from low to high by each described calibrating gas, and utilizes chromatography with discharge ionization detector in described gas chromatograph to carry out detection to obtain described standard colors spectrogram.
5. assay method according to claim 4, is characterized in that, the step obtaining the concentration of each oxides of nitrogen in described standard model comprises:
Utilize described gas chromatograph to described standard model replication n time, obtain the concentration measurement of each oxides of nitrogen in described standard model, n >=2;
The n of oxides of nitrogen each in described standard model described concentration measurement is averaged, and using the concentration of described mean value corresponding oxides of nitrogen in described standard model.
6. assay method according to claim 5, is characterized in that, described standard model is made up of with the volume ratio of 1:1 the first calibrating gas and the second calibrating gas; Described in described first calibrating gas, the concentration of NO is 5ppm, described N
2the concentration of O is 5ppm; Described in described second calibrating gas, the concentration of NO is 1ppm, described N
2the concentration of O is 1ppm; 2≤n>=5.
7. assay method according to claim 1, is characterized in that, in the correction factor=described standard model of each described oxides of nitrogen each oxides of nitrogen concentration/described standard model in the peak area of corresponding oxides of nitrogen.
8. assay method according to claim 1, is characterized in that,
Described gas to be measured comprises hydrogen, oxygen and carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon;
Test to described gas to be measured the step obtaining described test color spectrogram to comprise:
Described gas to be measured is passed in the pre-column of described gas chromatograph, component separation is carried out after utilizing heartcut principle to make described gas to be measured enter described pre-column, and peak sequence is hydrogen, oxygen and carbon monoxide, methane, carbon dioxide, oxides of nitrogen and hydrocarbon, after described oxides of nitrogen enters separating column from described pre-column outflow, by other component from atmospheric valve emptying;
Utilize that the separating column in described gas chromatograph and chromatography with discharge ionization detector are separated, the oxides of nitrogen detected in described gas to be measured, and obtain described test color spectrogram.
9. assay method according to claim 8, is characterized in that, tests the step that the step that obtains described test color spectrogram comprises comprise described gas to be measured:
Step S1, open sample introduction valve, make each component in described gas to be measured flow into described pre-column, make each component carry out pre-separation;
Step S2, treat that each described oxides of nitrogen in described gas to be measured flows out from described pre-column, flow into transfer valve after described separating column, make other impurity composition blowback emptying;
Be separated successively with the method for described step S2 according to described step S1, each described oxides of nitrogen detected in described gas to be measured, obtain the described test color spectrogram of each described oxides of nitrogen.
10. assay method according to claim 1, is characterized in that, the sensitivity of described gas chromatograph is less than 10mg/m
3.
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| CN114062540A (en) * | 2021-11-05 | 2022-02-18 | 中国测试技术研究院化学研究所 | Method for rapidly measuring impurity gases of oxygen and argon in pure gas |
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| CN111650294A (en) * | 2020-05-12 | 2020-09-11 | 中国核电工程有限公司 | Method for analyzing nitrogen oxide containing high-valence nitrogen |
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| CN114428121B (en) * | 2020-09-09 | 2024-04-09 | 中国石油化工股份有限公司 | High-concentration H 2 S-type natural gas full-component quantitative detection device and method |
| CN114062540A (en) * | 2021-11-05 | 2022-02-18 | 中国测试技术研究院化学研究所 | Method for rapidly measuring impurity gases of oxygen and argon in pure gas |
| CN114062540B (en) * | 2021-11-05 | 2024-05-03 | 中国测试技术研究院化学研究所 | Method for rapidly determining impurity gases oxygen and argon in pure gas |
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