CN110132949A - The method for measuring cement plant flue gas the escaping of ammonia - Google Patents
The method for measuring cement plant flue gas the escaping of ammonia Download PDFInfo
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- CN110132949A CN110132949A CN201910338606.9A CN201910338606A CN110132949A CN 110132949 A CN110132949 A CN 110132949A CN 201910338606 A CN201910338606 A CN 201910338606A CN 110132949 A CN110132949 A CN 110132949A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention discloses it is a kind of measure cement plant flue gas the escaping of ammonia method, comprising: cement plant flue gas is passed through into absorbing liquid, with after water constant volume prepare liquid;Prepare calibration curve solution;The prepare liquid and calibration curve solution are respectively placed in different color-comparison tubes, after water constant volume, it is mixed after being successively separately added into salicylic acid-citric acid three sodium solution, sodium nitroprusside solution and liquor natrii hypochloritis into each color-comparison tube, then each color-comparison tube is stablized into 2~4h in 30~40 DEG C, further according to the coloring depth, colorimetric assay obtains the concentration of cement plant ammonia in flue gas.The present invention measures ammonia density using indigo spectrophotometry, is not required to using the determination method by large-sized analytic instrument equipment, simple, quick, accurate, and save the cost has obvious practicability, is suitable for field laboratory analysis;Testing result is stablized, and favorable reproducibility improves accuracy, the precision of detection, and concentration range can be surveyed by having widened sample.
Description
Technical field
The invention belongs to testing fields, and in particular to a method of measurement cement plant flue gas the escaping of ammonia.
Background technique
Ammonia is unique alkaline gas in atmosphere, water-soluble, is chemically reacted with acidic materials, it is such chemically
Matter can be with sulfur dioxide, the nitrogen oxides (NO in atmosphereX) react the secondary aerosol species such as generation ammonium nitrate, ammonium sulfate.
Secondary aerosol species are the important sources of PM2.5, influence air quality, make environmental degradation, and therefore, the emission control of ammonia is worth closing
Note.
With the sustainable development of China's cement sectors, fine grained caused by nitrogen oxides and ozone layer pollution problem are increasingly tight
Weight, not only causes serious harm to environment, also brings threat to the physical and mental health of the mankind, the discharge for reducing nitrogen oxides becomes
It needs urgently to solve the problems, such as.Although the cement plant denitration technology and technique in current China gradually domesticize, in measurement ammonia
It is not also very mature that escape, which uses technically,.Currently, in order to control the discharge of nitrogen oxides, the out of stock skill master in domestic cement plant
If using SNCR technique, but the practice of this denitration technology is not grown, and experience is also insufficient, and the escaping of ammonia phenomenon is serious.Therefore, it grinds
Studying carefully the out of stock the escaping of ammonia measurement application in new cement plant becomes current most urgent task.
Summary of the invention
Goal of the invention: aiming at the problems existing in the prior art, the present invention provides a kind of stabilizations, Accurate Determining cement plant
The method of flue gas such as SNCR technique flue gas the escaping of ammonia.
Technical solution: the method for present invention measurement cement plant flue gas the escaping of ammonia, comprising:
(1) cement plant flue gas is passed through into absorbing liquid, with after water constant volume prepare liquid;
(2) calibration curve solution is prepared;
(3) prepare liquid and calibration curve solution are respectively placed in different color-comparison tubes, after water constant volume,
Salicylic acid-citric acid three sodium solution, sodium nitroprusside solution and hypochlorous acid are successively separately added into each color-comparison tube
Mixed after sodium solution, each color-comparison tube then stablized into 2~4h in 30~40 DEG C, further according to coloring the depth, colorimetric assay,
Obtain the concentration of cement plant ammonia in flue gas.
The absorbing liquid is the aqueous sulfuric acid of 0.004~0.006mol/L of concentration, is absorbed twice, when absorbing every time
Absorbing liquid volume be 30~50ml;Preferably, the absorbing liquid is the aqueous sulfuric acid of concentration 0.005mol/L.
In step (1), it is settled to 100ml.
The flow that cement plant flue gas is passed through into absorbing liquid is 4~5L/min, and being passed through the time is 0.6~10min, cement plant
Flue gas sampling belongs to stench source sampling, and the absorbing liquid volume absorbed every time is 30~50mL, selects this flow and time, is two
Combined factors consider that general gas flow sampling pump is L/min, and when pump discharge is too big, the sampling time especially in short-term, flows through 30~50mL
Absorbing liquid when, ammonia absorb not exclusively, have part have little time absorb just with gas discharge absorption bottle outside, calculate sample when
Between when, also have certain error, error is too big when flow is too big.On the contrary, gas has absorbed when gas sampling pump discharge is too small
Entirely, but the sampling time can increase significantly, need to do the repeated experiment of multiple repairing weld at the scene, comparatively laborious.First and
The last one sampling meeting interval time is longer, is also unfavorable for the requirement analyzed as early as possible after subsequent sampling.4~5L/min of sampling flow
When, the bubble that gas flows through absorbing liquid is more uniform, and the comparison that ammonia absorbs is complete, and the sampling time is more reasonable, is especially adopting
When sample number is more, be conducive to subsequent experimental analysis.Preferably, the flow that cement plant flue gas is passed through into absorbing liquid is 5L/
Min, being passed through the time is 3~5min.
In step (2), calibration curve solution is prepared using ammonium chloride.
In step (3), 10ml is settled to water in color-comparison tube.
The concentration of the salicylic acid-citric acid three sodium solution is 45~50g/L, and additional amount is 0.5~0.6mL;Nitroso
The concentration of sodium ferricyanide solution is 8~10g/L, and additional amount is 0.1~0.15mL;The concentration of liquor natrii hypochloritis be 0.04~
0.05mol/L, additional amount are 0.1~0.15mL.Preferably, the concentration of the salicylic acid-citric acid three sodium solution is 50g/L,
Additional amount is 0.5mL;The concentration of sodium nitroprusside solution is 10g/L, additional amount 0.1mL;Liquor natrii hypochloritis's is dense
Degree is 0.05mol/L, additional amount 0.1mL.
The determination of the upper limit of the method for the present invention ammonia is 50mg/m3, Determination Limit 0.01mg/m3。
The present invention has the following advantages and beneficial to effect compared with the existing technology according to the on-site actual situations in cement plant
Fruit:
The present invention measures ammonia density using indigo spectrophotometry, it is determined that colour temp, developing time and color developing agent
The influence to analysis result such as dosage.It is not required to using the determination method by large-sized analytic instrument equipment, simple, quick,
Accurately, save the cost has obvious practicability, is suitable for field laboratory analysis, and the environmental protection for the following cement denitration engineering is tested
It receives and Performance Assessment provides reference.
Steps are as follows for indophenol blue chromogenic reaction:
Indophenol blue chromogenic reaction is that a kind of mechanism is more complex, the chemical reaction that substep carries out.First step ammonia and dilute sulfuric acid are anti-
Ammonium ion should be formed;Second step ammonium ion and sodium hypochlorite reaction generate chloramines;Third step chloramines and salicylic acid are in alkaline environment
Lower reaction generates intermediate product -5-aminosalicylic acid, is quickly oxidized again generates 2 carboxyls-Isosorbide-5-Nitrae quinone imines later;4th step with
Sodium nitroprusside is catalyst, and 2 carboxyls-Isosorbide-5-Nitrae quinone imines and salicylic acid, which further react, generates glaucous indophenols.
The reaction has catalyst addition, illustrates that reaction is a long response time, is added after catalyst and one dynamically balances
Reaction, has no specific reaction end.Consulting literatures data does not find the behavioral illustrations data more about the reaction.
In previous research or national standard, saved at room temperature after sample, then plus color developing agent carries out reaction balance, and
Some researches show that reaction temperatures not to influence on final detection result, however inventor sends out in the detection to flue gas the escaping of ammonia
Existing, according to previous condition, the linear dependence of standard curve is poor, and highly unstable, it is difficult to the concentration of accurate detection ammonia, because
This, inventor promotes temperature, can not only the reaction time be made to shorten, and substantially increase the linear dependence of standard curve, examines
It surveys result to stablize, favorable reproducibility improves accuracy, the precision of detection, and concentration range can be surveyed by having widened sample.
Detailed description of the invention
Fig. 1 is the gas absorbing device that the method for the present invention uses;
Fig. 2 is 1 standard curve of embodiment;
Fig. 3 is 2 standard curve of embodiment;
Fig. 4 is 3 standard curve of embodiment.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention
The modification of form falls within the application range as defined in the appended claims.
The reagent that following specific embodiments use is as follows:
Salicylic acid-citric acid three sodium solution: salicylic acid solution concentration 50g/L weighs 5.0g salicylic acid [C6H4(OH)COOH]
With 5.0g sodium citrate (Na3C6H5O7·2H2O), add water 25mL, then plus 22.5mL sodium hydroxide solution [c (NaOH)=2mol/
L], it is diluted with water to 100mL.
Sodium nitroprusside solution: sodium nitroprusside concentration 10g/L weighs 1.0g sodium nitroprusside
[Na2Fe(CN)5·NO·2H2O], it is dissolved in 100mL water.
Liquor natrii hypochloritis: liquor natrii hypochloritis concentration 0.05mol/L demarcates its concentration with iodimetric titration, uses sodium hydroxide
Solution [c (NaOH)=2mol/L] is diluted to the solution of 0.05mol/L.
Specific step is as follows for iodimetric titration calibration sodium hypochlorite concentration: weighing 2g potassium iodide in 250mL iodine flask, adds water
50mL dissolution, adds 1.0mL sodium hypochlorite reagent, then plus 0.5mL hydrochloric acid solution [50% (V/V)], shake up, 3min is placed in dark place.
With sodium thiosulfate standard solution [c (1/2Na2S2O3)=0.1mol/L].Iodine is precipitated in titration, until adding when solution is in yellow
The starch indicator (5g/L) that 1mL is newly prepared continues to be titrated to blue and just takes off, as terminal, notes down thiosulfuric acid used
Sodium solution volume calculates the concentration of liquor natrii hypochloritis.
C (NaClO)=c (1/2Na2S2O3)×V/2
In formula: c (NaClO)-sodium hypochlorite reagent concentration, mol/L;
c(1/2Na2S2O3)-Concentration of Sodium Thiohsulfate Standard Solution, mol/L;
V- sodium thiosulfate standard solution dosage, mL.
The device that following embodiments use when absorbing flue gas with absorbing liquid is as shown in Figure 1, include two using beam ground
Absorption bottle, volume 100ml is respectively designated as the first absorption bottle 1 and the second absorption bottle 2;The end of smoke collecting pipe 3 is protruded into
In absorbing liquid in first absorption bottle 1, for conveying flue gas into the first absorption bottle;First absorption bottle the top of absorbing liquid also
It is connected with the communicating pipe 4 that end is protruded into the second absorption bottle absorbing liquid, the second absorption bottle 2 is equipped with evacuated tube in the top of absorbing liquid
5。
When sampling, flue gas is passed through smoke collecting pipe (can be such as passed through flue gas by sampling pump), flue gas is inhaled by first
After the absorbing liquid absorbing ammonia for receiving bottle, into the second absorption bottle, remaining ammonia is absorbed by the absorbing liquid of the second absorption bottle, has been absorbed
Full flue gas is discharged by evacuated tube, after sampling after a period of time, by the absorption in the first absorption bottle and the second absorption bottle
Liquid mixing.
Embodiment 1
The glass apparatus such as colorimetric cylinder, pipette used in simultaneously flash baking are cleaned before experiment.It is logical with sampling pump control flue gas
The flow for crossing smoke collecting pipe is 5L/min, and the gas production time is 3.6min.Cement plant flue gas is by concentration by the sulphur of 0.005mol/L
Acid solution (absorbing liquid) fully absorbs, and the volume of sulfuric acid is 30mL in each absorption bottle, by the suction in two absorption bottles after absorption
Liquid is received to merge and be settled to 100mL with water.
Prepare calibration curve solution: standard curve solution concentration is 1 μ g ammonia/mL, prepares to obtain by ammonium chloride plus water.
Absorbing liquid after 0~10ml calibration curve solution and 1ml to be absorbed to flue gas is respectively placed in different 10mL tool plugs
In colorimetric cylinder.Each colorimetric cylinder is diluted with water to 10mL scale, be sequentially added into 0.5mL salicylic acid-citric acid three sodium solution,
0.1mL sodium nitroprusside solution and 0.1mL sodium hypochlorite use liquid, shake up.Each colorimetric cylinder is placed in 32 DEG C of baking ovens
Stablize 4h, according to the coloring depth, (spectrophotometer measures absorbance to colorimetric assay at wavelength 697.5nm, according to absorbance meter
Calculate ammonia content).According to ammonia content in solution, the testing result for obtaining cement plant flue gas the escaping of ammonia is 8mg/m3.Fig. 2 is this implementation
The standard curve of example, R2=0.9992.
Embodiment 2
The glass apparatus such as colorimetric cylinder, pipette used in simultaneously flash baking are cleaned before experiment.It is logical with sampling pump control flue gas
The flow for crossing smoke collecting pipe is 5L/min, and the gas production time is 1min.Cement plant flue gas is by concentration by the sulfuric acid of 0.005mol/L
Solution fully absorbs, and the volume of sulfuric acid is 50mL in each absorption bottle, merges the absorbing liquid in two absorption bottles simultaneously after absorption
100mL is settled to water.
Prepare calibration curve solution: standard curve solution concentration is 1 μ g ammonia/mL, prepares to obtain by ammonium chloride plus water.
Absorbing liquid after 0~10ml calibration curve solution and 5.5ml to be absorbed to flue gas is respectively placed in different 10mL tools
It fills in colorimetric cylinder.Each colorimetric cylinder is diluted with water to 10mL scale, be sequentially added into 0.5mL salicylic acid-citric acid three sodium solution,
0.1mL sodium nitroprusside solution and 0.1mL sodium hypochlorite use liquid, shake up.Each colorimetric cylinder will be placed in 40 DEG C of baking ovens
Middle stable 2h, according to the coloring depth, colorimetric assay.According to ammonia content in solution, the detection knot of cement plant flue gas the escaping of ammonia is obtained
Fruit is 30mg/m3.Fig. 3 is the standard curve of the present embodiment, R2=0.9986.
Comparative example 1
Absorbing liquid after 0~10ml calibration curve solution and 1ml that 1 method of embodiment obtains to be absorbed to flue gas is placed respectively
In different 10mL color-comparison tubes.Each colorimetric cylinder is diluted with water to 10mL scale, is sequentially added into 0.5mL salicylic acid-
Citric acid three sodium solution, 0.1mL sodium nitroprusside solution and 0.1mL sodium hypochlorite use liquid, shake up.By each ratio when winter
Colour tube is placed in middle stable 1h at 15 DEG C of room temperature, according to the coloring depth, colorimetric assay.It was found that the linear dependence of standard curve becomes
Difference, is 0.9114, cannot still improve linear dependence by the time such as 12h that extend stable.
Claims (8)
1. a kind of method for measuring cement plant flue gas the escaping of ammonia characterized by comprising
(1) cement plant flue gas is passed through into absorbing liquid, with after water constant volume prepare liquid;
(2) calibration curve solution is prepared;
(3) prepare liquid and calibration curve solution are respectively placed in different color-comparison tubes, after water constant volume, to each
It is molten that salicylic acid-citric acid three sodium solution, sodium nitroprusside solution and sodium hypochlorite are successively separately added into color-comparison tube
It is mixed after liquid, each color-comparison tube is then stablized into 2~4h in 30~40 DEG C, further according to the coloring depth, colorimetric assay is obtained
The concentration of cement plant ammonia in flue gas.
2. the method for measurement cement plant flue gas the escaping of ammonia according to claim 1, which is characterized in that the absorbing liquid is
The aqueous sulfuric acid of 0.004~0.006mol/L of concentration is absorbed twice, every time absorb when absorbing liquid volume be 30~
50ml。
3. the method for measurement cement plant flue gas the escaping of ammonia according to claim 1, which is characterized in that in step (1), constant volume
To 100ml.
4. the method for measurement cement plant flue gas the escaping of ammonia according to claim 1, which is characterized in that be passed through into absorbing liquid
The flow of cement plant flue gas is 4~5L/min, and being passed through the time is 0.6~10min.
5. the method for measurement cement plant flue gas the escaping of ammonia according to claim 1, which is characterized in that prepared using ammonium chloride
Calibration curve solution.
6. the method for measurement cement plant flue gas the escaping of ammonia according to claim 1, which is characterized in that in step (3), having
10ml is settled to water in plug colorimetric cylinder.
7. the method for measurement cement plant flue gas the escaping of ammonia according to claim 1, which is characterized in that salicylic acid-citric acid
The concentration of three sodium solutions is 45~50g/L, and additional amount is 0.5~0.6mL;The concentration of sodium nitroprusside solution be 8~
10g/L, additional amount are 0.1~0.15mL;The concentration of liquor natrii hypochloritis be 0.04~0.05mol/L, additional amount be 0.1~
0.15mL。
8. the method for measurement cement plant flue gas the escaping of ammonia according to claim 1, which is characterized in that the determination of the upper limit of ammonia is
50mg/m3, Determination Limit 0.01mg/m3。
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Cited By (2)
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CN111693477A (en) * | 2020-05-20 | 2020-09-22 | 华南理工大学 | Product detection method of organic electrochemical synthesis ammonia reaction system |
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