CN110487781A - A kind of detection method of nitrogen oxides - Google Patents
A kind of detection method of nitrogen oxides Download PDFInfo
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- CN110487781A CN110487781A CN201910631929.7A CN201910631929A CN110487781A CN 110487781 A CN110487781 A CN 110487781A CN 201910631929 A CN201910631929 A CN 201910631929A CN 110487781 A CN110487781 A CN 110487781A
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Abstract
The present invention relates to a kind of detection methods of nitrogen oxides, which comprises the steps of: S1: preparing stock solution: S2: preparing developing solution；S3: preparation absorbing liquid, and the absorbance of absorbing liquid is detected, it is calculated as A0；S4: nitrogen oxides specimen sample；S5: drawing the nitrogen oxides sample in S4 with big tripe pipette, mix constant volume with the absorbing liquid in S3, after color presentation brownish red, carries out colorimetric detection with visible spectrophotometer after room temperature puts dark place 20 to 30 minutes, obtains standard specimen absorbance, be calculated as A1；S6: standard working curve figure is drawn, standard curve intercept a and slope of standard curve b are obtained；S7: the concentration of nitrogen oxides is calculated using formula.Method fairly simpleization of the invention, understandable easy to operate, save the cost.Do not allow error-prone when analysis, detection data relatively standard value, numerical value is more acurrate, and precision is higher, more effective to improve experiment operational efficiency.
Description
Technical field
The present invention relates to NOx sensing technologies field more particularly to a kind of detection methods of nitrogen oxides.
Background technique
Nitrogen oxides (NOX) in surrounding air is mainly the chemical combination that nitric oxide (NO) and nitrogen dioxide (NO2) are formed
Object.Nitrogen oxides can indirectly form acid rain, and generate the main component of vehicle exhaust.In view of various danger of nitrogen oxides
Evil property, it is necessary to the measurement of amount of nitrogen oxides is carried out, to understand and grasp the concentration feelings of nitrogen oxides in air in region
Condition carries out the evaluation of air quality, and atmospheric environment and human health is avoided to be encroached on.
National standard measuring method, but the step of national standard measuring method are generallyd use in nitrogen oxides context of detection at present
The disadvantages of rapid comparatively laborious, it is bigger that there are monitoring data deviations, is unfavorable for fast operating.
Summary of the invention
It is an object of the invention to make up the defect of technology existing for existing national standard measuring method, a kind of nitrogen oxygen is provided
The new detecting method of compound.
For achieving the above object, the technical scheme adopted by the invention is as follows: a kind of detection method of nitrogen oxides, it is special
Sign is, includes the following steps: S1: prepare stock solution: after (N-1- naphthalene) ethylenediamine-hydrochloride is diluted with distilled water, and constant volume
Into volumetric flask；S2: prepare developing solution: cooling reaches room temperature after p-aminobenzene sulfonic acid is dissolved in low-grade fever distilled water,
Constant volume is carried out with distilled water after the stock solution and glacial acetic acid that are separately added into S1, is fitted into the reagent bottle of brown after shaking uniformly；S3:
Preparation absorbing liquid: by S2 developing solution and distilled water be mixed in a certain ratio and to form nox adsorption liquid, and measure absorption
The absorbance of liquid, is calculated as A0；S4: nitrogen oxides specimen sample: the gas containing nitrogen oxides is passed sequentially through containing inhaling in S3
Receive the first porous glass plate absorption bottle, the oxygen cylinder containing liquor potassic permanganate and the second porous containing absorbing liquid in S3 of liquid
Plate absorption bottle, wherein the solution in the second porous glass plate absorption bottle is nitrogen oxides sample；S5: S4 is drawn with big tripe pipette
In nitrogen oxides sample, mix constant volume with the absorbing liquid in S3, after color present brownish red after, put dark place 20 to 30 in room temperature
Colorimetric detection is carried out with visible spectrophotometer after minute, standard specimen absorbance is obtained, is calculated as A1；S6: standard working curve is drawn
Figure, obtains standard curve intercept a and slope of standard curve b；S7: the concentration for calculating nitrogen oxides is as follows: nitrogen oxidation nitrogen concentration=
(A1-A0-a)/b, in which: the unit of nitrous oxides concentration is mg/m3.
Further, in S1, the weight of (N-1- naphthalene) ethylenediamine-hydrochloride is 0.2500g, and the capacity after constant volume is
250mL。
Further, in S2, the weight of aminobenzenesulfonic acid is 2.50g, and low-grade fever distilled water is 100mL, stock solution 25mL,
Glacial acetic acid is 25mL, and constant volume capacity is 500mL.
Further, it in S2, is packed into after the reagent bottle of brown to seal and is stored in refrigerator, storage life is 3 months.
Further, in S3, developing solution and distilled water are mixed in the ratio of 4:1, and the absorbance of absorbing liquid is not more than
0.005。
Further, in S4, the absorbing liquid in the first porous glass plate absorption bottle and the second porous glass plate absorption bottle is 10 mL
；Liquor potassic permanganate is 10 mL in oxygen cylinder；Gas flow 0.4L/min containing nitrogen oxides, the gas containing nitrogen oxides
Body volume is 20L.
Further, in S5, the nitrogen oxides sample that big tripe pipette is drawn is 10.00mL, the appearance with absorbing liquid constant volume
Product is 250mL, and room temperature is not less than 20 degree.
Beneficial effects of the present invention: method fairly simpleization of the invention, understandable easy to operate, save the cost.When analysis not
It is easy error, detection data relatively standard value, numerical value is more acurrate, and precision is higher, more effective to improve experiment operational efficiency.
Detailed description of the invention
Fig. 1 is the standard working curve figure in embodiment.
Specific embodiment
Principle: the present invention is made into absorbing liquid using glacial acetic acid, p-aminobenzene sulfonic acid and hydrochloride naphthodiamide.Atmosphere when sampling
In NO X Finally with NO after absorbing liquid and potassium permanganate are easy 2 Form be absorbed, generate nitrous acid and nitric acid, then
Diazo-reaction is played with the p-aminobenzene sulfonic acid in absorbing liquid, is finally coupled with hydrochloride naphthodiamide, generates the azo of brownish red
NO in compound, shade and gas sample 2 Concentration is directly proportional, to pass through the amount of spectrophotometry solution nitrite
To calculate the levels of nitrogen oxides indirectly.
Embodiment: the experimental facilities (article) that the present embodiment uses specifically includes that national standard sample nitrogen oxides (water
Agent), lot number: 206148, standard value: 0.255 ± 0.017, unit: mg/L, specification: 20mL ampulla；722 type visible spectrophotometrics
Meter, colorimetric wavelength: 540nm；Colorimetric cylinder: 10mL；Brown volumetric flask: cuvette: 1cm；Distilled water；Glacial acetic acid (purity 95%)；
(N-1- naphthalene) ethylenediamine-hydrochloride；P-aminobenzene sulfonic acid.
Experimental solutions: hydrochloride naphthodiamide stock solution: precise 0.2500g(N-1- naphthalene) ethylenediamine-hydrochloride steaming
Distilled water is diluted to the volumetric flask of 250mL, is settled to graduation mark.Developing solution: weighing 2.50g and analyze pure p-aminobenzene sulfonic acid, with big
The low-grade fever distilled water of about 100mL dissolves, and reaches room temperature to the cooling of amino phenyl sulfonyl acid solution.Then amino phenyl sulfonyl acid solution all moves
The volumetric flask for entering 500mL is separately added into 25mL hydrochloride naphthodiamide stock solution and 25mL glacial acetic acid, is settled to scale with distilled water
Line shakes uniformly.It is packed into the reagent bottle of brown, sealing in storing in refrigerator, is valid for three months.If the developing solution of preparation goes out
Existing pale red, illustrates contaminated, and what should be abandoned prepares developing solution again.Absorbing liquid: developing solution and distilled water press the ratio of 4:1
Example mixes.The absorbing liquid that (now matching when experiment) prepares should measure absorbance, be calculated as A0, and the absorbance A of absorbing liquid0It cannot
Greater than 0.005, if it exceeds 0.005, should check whether the reagent of preparation is qualified, and whether reagent purity is up to standard, laboratory distillation
Whether water is up to standard, and whether developing solution preservation is eligible etc..
Analysis method: using national standard method and detection method of the invention respectively to the national standard sample in embodiment
Product nitrogen oxides (aqua) is detected, to prove the technical effect of the method for the present invention by data comparison.The present embodiment
In, 10.00mL national standard sample nitrogen oxides (aqua) is accurately drawn using big tripe pipette, it is direct with absorbing liquid obtained
For constant volume to 250mL, brownish red is presented in color, dark place is put 20 minutes with the room temperature not less than 20 degree, with 722 type visible spectrophotometrics
Colorimetric detection is counted, the absorbance of standard specimen is measured, is calculated as A1, the standard working curve drawn is as shown in Figure 1, standard curve
Intercept is calculated as a；The slope of standard curve is calculated as b, is then calculated by formula nitrogen oxidation nitrogen concentration=(A1-A0-a)/b
The concentration of nitrogen oxides.Wherein: the unit of nitrous oxides concentration is mg/m3, the absorbance of absorbing liquid is calculated as A0；Standard specimen extinction
Degree, is calculated as A1；
Conclusion: by using national standard method and detection method of the invention to national standard sample nitrogen oxides (water twice
Agent) detection comparison is carried out, wherein national standard method absorbance is 0.056,0.055.Testing result is respectively 0.247,
0.242.Average value is 0.244, relative standard deviation 1.45%.Use the absorbance of detection method of the invention for 0.257,
0.256, testing result is respectively 0.256,0.255, average value 0.256, relative standard deviation 0.28%.It is possible thereby to
Out: national standard measuring method, step is comparatively laborious, and monitoring data deviation is bigger, detection method of the invention, understandable easy behaviour
Make, save the cost, when analysis does not allow error-prone, detection data relatively standard value, for opposite national standard measuring method
Standard deviation is smaller, and numerical value is more acurrate, and precision is higher.So analyzing nitrogen oxides standard sample with detection method of the invention
Product can more embody analysis data accuracy, reasonability etc., more effective to improve experiment operational efficiency.
Claims (7)
1. a kind of detection method of nitrogen oxides, which comprises the steps of:
S1: prepare stock solution: after (N-1- naphthalene) ethylenediamine-hydrochloride is diluted with distilled water, constant volume is into volumetric flask；
S2: prepare developing solution: cooling reaches room temperature after p-aminobenzene sulfonic acid is dissolved in low-grade fever distilled water, is separately added into
Constant volume is carried out with distilled water after stock solution and glacial acetic acid in S1, is fitted into the reagent bottle of brown after shaking uniformly；
S3: preparation absorbing liquid: by S2 developing solution and distilled water be mixed in a certain ratio and to form nox adsorption liquid, and survey
The absorbance for determining absorbing liquid, is calculated as A0；
S4: it is porous that the gas containing nitrogen oxides nitrogen oxides specimen sample: is passed sequentially through first containing absorbing liquid in S3
Glass plate absorption bottle, the oxygen cylinder containing liquor potassic permanganate and the containing absorbing liquid in S3 second porous glass plate absorption bottle, wherein
Solution in second porous glass plate absorption bottle is nitrogen oxides sample；
S5: drawing the nitrogen oxides sample in S4 with big tripe pipette, mix constant volume with the absorbing liquid in S3, and palm fibre is presented to color
After red, colorimetric detection is carried out with visible spectrophotometer after room temperature puts dark place 20 to 30 minutes, obtains standard specimen absorbance, is counted
For A1；
S6: standard working curve figure is drawn, standard curve intercept a and slope of standard curve b are obtained；
S7: the concentration for calculating nitrogen oxides is as follows:
Nitrous oxides concentration=(A1-A0- a)/b, in which: the unit of nitrous oxides concentration is mg/m3。
2. a kind of detection method of nitrogen oxides according to claim 1, which is characterized in that in S1, (N-1- naphthalene) second
The weight of diamine hydrochloride is 0.2500g, and the capacity after constant volume is 250mL.
3. a kind of detection method of nitrogen oxides according to claim 2, which is characterized in that in S2, aminobenzenesulfonic acid
Weight is 2.50g, and low-grade fever distilled water is 100mL, stock solution 25mL, glacial acetic acid 25mL, and constant volume capacity is 500mL.
4. a kind of detection method of nitrogen oxides according to claim 3, which is characterized in that in S2, be packed into the examination of brown
Sealing is stored in refrigerator after agent bottle, and storage life is 3 months.
5. a kind of detection method of nitrogen oxides according to claim 3, which is characterized in that in S3, developing solution and distillation
Water is mixed in the ratio of 4:1, and the absorbance of absorbing liquid is not more than 0.005.
6. a kind of detection method of nitrogen oxides according to claim 5, which is characterized in that in S4, the first porous glass plate
Absorbing liquid in absorption bottle and the second porous glass plate absorption bottle is 10 mL；Liquor potassic permanganate is 10 mL in oxygen cylinder；Contain
The gas flow 0.4L/min of nitrogen oxides, the gas volume containing nitrogen oxides are 20L.
7. a kind of detection method of nitrogen oxides according to claim 6, which is characterized in that in S5, big tripe pipette is inhaled
The nitrogen oxides sample taken is 10.00mL, and the volume with absorbing liquid constant volume is 250mL, and room temperature is not less than 20 degree.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111289501A (en) * | 2020-02-21 | 2020-06-16 | 安徽大千生物工程有限公司 | Kit for detecting NO based on indirect colorimetric method and preparation and use methods thereof |
| CN112697532A (en) * | 2021-01-08 | 2021-04-23 | 杨松 | Sampling method for nitrogen oxides in ambient air |
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| US20090128819A1 (en) * | 2005-04-26 | 2009-05-21 | Koninklijke Philips Electronics, N.V. | Low cost apparatus for detection of nitrogen-containing gas compounds |
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2019
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Patent Citations (4)
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| US20090128819A1 (en) * | 2005-04-26 | 2009-05-21 | Koninklijke Philips Electronics, N.V. | Low cost apparatus for detection of nitrogen-containing gas compounds |
| CN101013092A (en) * | 2007-01-31 | 2007-08-08 | 山东建筑大学 | Indoor air quality rapid determination instrument and determination method thereof |
| CN105021607A (en) * | 2015-08-18 | 2015-11-04 | 中国神华能源股份有限公司 | Determination device and determination method for determining nitric oxide content in liquid oxygen |
| CN207570864U (en) * | 2017-12-21 | 2018-07-03 | 山东鼎安检测技术有限公司 | A kind of nitrogen oxides on-site detecting device |
Non-Patent Citations (1)
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| 环境保护部: "《环境空气 氮氧化物（一氧化氮和二氧化氮）的测定 盐酸萘乙二胺分光光度法 HJ 479－2009》", 27 September 2009 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111289501A (en) * | 2020-02-21 | 2020-06-16 | 安徽大千生物工程有限公司 | Kit for detecting NO based on indirect colorimetric method and preparation and use methods thereof |
| CN112697532A (en) * | 2021-01-08 | 2021-04-23 | 杨松 | Sampling method for nitrogen oxides in ambient air |
| CN112697532B (en) * | 2021-01-08 | 2022-09-13 | 挪亚检测技术有限公司 | Sampling method for nitrogen oxides in ambient air |
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Application publication date: 20191122 |