CN111751363A - Quantitative testing device and testing method for ammonia nitrogen substances in fly ash - Google Patents
Quantitative testing device and testing method for ammonia nitrogen substances in fly ash Download PDFInfo
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- CN111751363A CN111751363A CN202010567912.2A CN202010567912A CN111751363A CN 111751363 A CN111751363 A CN 111751363A CN 202010567912 A CN202010567912 A CN 202010567912A CN 111751363 A CN111751363 A CN 111751363A
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- 239000010881 fly ash Substances 0.000 title claims abstract description 66
- 238000012360 testing method Methods 0.000 title claims abstract description 35
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000000126 substance Substances 0.000 title claims abstract description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000007788 liquid Substances 0.000 claims abstract description 75
- 238000010521 absorption reaction Methods 0.000 claims abstract description 67
- 238000004821 distillation Methods 0.000 claims abstract description 59
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000004448 titration Methods 0.000 claims abstract description 37
- 238000000926 separation method Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000012113 quantitative test Methods 0.000 claims abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 41
- 239000000523 sample Substances 0.000 claims description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 31
- 238000009825 accumulation Methods 0.000 claims description 23
- 238000010992 reflux Methods 0.000 claims description 21
- 239000006096 absorbing agent Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000005485 electric heating Methods 0.000 claims description 15
- 239000003513 alkali Substances 0.000 claims description 13
- 238000009833 condensation Methods 0.000 claims description 11
- 230000005494 condensation Effects 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000011229 interlayer Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000012086 standard solution Substances 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000005259 measurement Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000012496 blank sample Substances 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000010998 test method Methods 0.000 abstract description 4
- 239000004566 building material Substances 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 6
- 235000019270 ammonium chloride Nutrition 0.000 description 6
- 239000004567 concrete Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000007789 sealing Methods 0.000 description 4
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 description 4
- 239000004568 cement Substances 0.000 description 3
- 239000002274 desiccant Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000010795 Steam Flooding Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- -1 ammonium ions Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
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Abstract
The invention discloses a quantitative test device and a test method for ammonia nitrogen substances in fly ash, wherein the device comprises a distillation unit for generating steam, a distillation tube, a separation unit for separating ammonia gas, an absorption unit and a titration metering unit, wherein the distillation unit is connected with the distillation tube and an anti-splash water-vapor separator arranged at the upper end of the distillation tube through a steam pipeline, one end of the separation unit is connected with the upper end of the anti-splash water-vapor separator, the other end of the separation unit is connected with the absorption unit, and the titration metering unit is used for titrating ammonia-containing liquid to be tested in the absorption unit; the testing method adopts a direct titration method to reduce the influence factors such as the concentration and the dosage of the absorption liquid, the PH of the liquid to be tested and the like, and improve the precision; the automatic design simplifies the operation process and reduces human errors. The invention has wide test range and strong applicability; the method has the advantages of few influencing factors, higher data accuracy, low test cost and the like, thereby having strong popularization and application values in the aspect of quick detection of the ammonia in the fly ash and other building material products.
Description
Technical Field
The invention relates to the technical field of building material detection, in particular to a quantitative testing device and a testing method for ammonia nitrogen substances in fly ash.
Background
The fly ash is a byproduct of combustion power generation of a coal-fired power plant, is applied to cement, mortar and concrete products for a long time, plays roles in reducing cost and improving efficiency and improves performance, and is an important cementing material. In recent years, in order to respond to national environmental protection requirements and reduce ammonia nitrogen substances discharged to the atmosphere by enterprises such as thermal power plants and the like, the coal-fired power plants successively carry out denitration modification on units, and in the operation of SCR and SNCR, ammonia is used for treating nitrogen oxides in flue gas and simultaneously causing residues of the ammonia nitrogen substances in fly ash, so that the fly ash subjected to denitration modification continuously generates a large amount of bubbles and is accompanied with sharp smell in the application process of cement concrete, the setting time is obviously prolonged or even not solidified, the concrete expands in volume and is even seriously expanded, the interior is loose and porous, the strength is reduced and the like, the deterioration of the performance of the cement concrete is caused, and the quality safety and the construction environment safety of a concrete structure are seriously threatened. Therefore, the quantitative determination of ammonia nitrogen in the denitration fly ash has important significance for the fly ash use and production enterprises to control the quality of raw materials, enhance the quality stability and search corresponding ammonia-containing limit values.
Due to the diversity of chemical forms and physical combination forms of ammonia nitrogen substances in the fly ash, the test of the ammonia nitrogen content of the fly ash has a plurality of difficulties. Usually, ammonium ions are extracted by methods such as soaking, suction filtration or centrifugal separation of a fly ash sample, and the method is difficult to ensure that ammonia nitrogen substances in the fly ash are completely dissolved and extracted, and on the other hand, Ca in the fly ash is difficult to avoid2+、Mg2+Ion and gel interference problems. Another test method refers to the distillation-titration method in GB18588 limit for Ammonia Release in concrete Admixture, which reducesThe interference of ions and gel, but the defects that the extraction efficiency of fly ash ammonia nitrogen is not high, the indirect titration result is easily influenced by multiple factors such as the dosage, concentration of the liquid to be detected, pH value and the like, the operation is complicated, the data fluctuation is large and the like exist.
Disclosure of Invention
Aiming at the problems, the invention provides a quantitative test device and a test method for ammonia nitrogen substances in fly ash, which adopt excessive alkali liquor reaction and steam drive to accelerate the overflow of ammonia gas and improve the separation efficiency of the ammonia gas; reflux cooling and drying separation are adopted to avoid introducing water vapor to dilute the solution to be tested; the method is combined with an absorber to efficiently absorb ammonia gas, and a direct titration method is adopted to reduce the influence factors such as the concentration, the dosage, the PH of the liquid to be detected and the like, so that the method is simple to operate and has high data accuracy and precision.
The invention adopts the following technical scheme:
a quantitative test device for ammonia nitrogen substances in fly ash comprises a distillation unit for generating steam, a distillation pipe, a separation unit for separating ammonia gas, an absorption unit and a titration metering unit, wherein the distillation unit is connected with the distillation pipe and an anti-splash water-vapor separator arranged at the upper end of the distillation pipe through a pipeline;
the splash-proof water-vapor separator comprises a front cavity and a rear cavity, a splash-proof disc is arranged above the front cavity, extends into the rear cavity and is communicated with the rear cavity, the splash-proof disc prevents reaction liquid from boiling over to enter a subsequent pipeline, a through hole is arranged between the front cavity and the rear cavity and serves as a backflow hole, heat-preservation interlayers are wrapped outside the front cavity and the rear cavity, and a steam inlet and a steam outlet are arranged on the heat-preservation interlayers; hot steam is introduced into the heat-insulating interlayer to improve the working temperature of the anti-splash steam separator, reduce the solubility of ammonia gas and improve the separation efficiency.
Preferably, the distillation unit comprises a steam generating bottle and an electric heating element arranged in the steam generating bottle, the electric heating element is an electric heating pipe, and the electric heating element heats distilled water in the steam generating bottle to generate hot steam.
Preferably, an alkali liquor reagent bottle and a sample chamber which are communicated with the inside of the distillation tube are arranged above the distillation tube, the alkali liquor reagent bottle is used for adding alkali liquor into the distillation tube, and the sample chamber is filled with the soaked coal ash sample.
Preferably, the separation unit comprises a reflux condensation pipe obliquely arranged at the upper end of the splash-proof water-vapor separator, and a dryer arranged at the right end of the reflux condensation pipe, wherein the reflux condensation pipe is used for reducing the temperature of the distilled gas to avoid introducing a large amount of water vapor into the absorption liquid, and the dryer is filled with an alkaline desiccant to further separate ammonia and water vapor and avoid introducing water vapor to greatly dilute the concentration of the ammonia-containing liquid to be detected.
Preferably, the absorption unit comprises a liquid accumulation bottle, an absorption liquid reagent bottle and an absorption pipeline, one end of the absorption pipeline is connected with the dryer, the other end of the absorption pipeline extends into the bottom of the liquid accumulation bottle, the bottom of the liquid accumulation bottle is provided with a parallel lens, and the absorption pipeline is provided with at least one absorber to improve the absorption efficiency of ammonia gas; and the absorption liquid reagent bottle is connected with the effusion bottle or the absorber through a pipeline.
Preferably, the titration metering unit comprises a magnetic stirrer for stirring the liquid accumulation bottle, a color recognition device for recognizing color change and judging an end point, a flow meter and a titration liquid reagent bottle, wherein a reagent in the titration liquid reagent bottle is pumped into the liquid accumulation bottle through a pump, and the consumption of the reagent is metered through the flow meter.
Preferably, the testing device further comprises an automatic integrated controller, wherein the automatic integrated controller is used for controlling the on-off of the electric heating element and controlling the on-off of the valve on the pipeline through a relay and a solenoid valve.
A test method of a quantitative test device for ammonia nitrogen substances in fly ash comprises the following steps:
s1, cleaning by using ammonia-free distilled water, connecting the device, weighing a certain mass of fly ash, filling the fly ash into a sample chamber (9), adding distilled water for soaking and washing, and allowing the fly ash to enter a distillation tube to keep the tightness of the device;
s2, under a closed state, firstly adding absorption liquid into the liquid accumulation bottle, then adding excessive alkaline reaction liquid into the distillation tube through the alkaline liquid reagent bottle, introducing hot steam generated by the distillation unit into the distillation tube and the anti-splash water-steam separator, and carrying out steam stripping distillation;
s3, after splash-proof water-vapor separation, condensation reflux and drying treatment, introducing the distillate gas into an absorption unit to be absorbed by absorption liquid to obtain liquid containing ammonia to be detected;
s4, adding a color indicator into the ammonia-containing solution to be detected, starting a magnetic stirrer for stirring, and dropwise adding a titration reagent with known concentration to a color change end point;
s5, calculating the content of ammonia nitrogen substances in the fly ash according to the consumption of the titration reagent, wherein the calculation formula of the ammonia content in the fly ash is as follows:
in the formula, X is the ammonia content of the fly ash, ppm; v2 is the volume of hydrochloric acid standard solution consumed by the test sample, ml; v0 is the volume, ml, of hydrochloric acid standard solution consumed by the measurement of the blank sample; m is the mass of the fly ash sample, g; c is the concentration of the titrated hydrochloric acid standard solution, mol/L.
Preferably, the alkaline reaction solution is sodium hydroxide or potassium hydroxide, the mass concentration is 5-50 wt%, and the mass ratio of the alkaline reaction solution to the fly ash sample is as follows: (5-50): (5-30);
the absorption liquid is boric acid, the mass concentration is 1.5-4 wt%, and the mass ratio of the absorption liquid to the fly ash sample is as follows: (20 to 200) and (5 to 30).
Preferably, the color indicator is a methyl red-methylene blue solution or a methyl red-bromophenol green mixed indicator, the titration reagent is a standard dilute hydrochloric acid or dilute sulfuric acid solution with a known concentration, and the concentration range is 0.001-0.1 mol/L; the ammonia-containing solution to be detected is mainly ammonium borate and excessive boric acid solution, a target product is directly titrated by using strong acid such as dilute hydrochloric acid or dilute sulfuric acid, and the titration of the weak acid and weak base salt of ammonium borate is not influenced by the pH of the titrated product, the concentration and the dosage of the absorption solution, so that interference factors are reduced, and the data stability is improved.
The invention has the beneficial effects that:
1. the separation unit of the invention adopts the anti-splash steam separator, the reflux condensing device and the drying device which are designed by interlayer heating, improves the separation efficiency of ammonia gas and solves the problem that the concentration of the liquid to be detected is greatly diluted by introducing steam; the ammonia gas is efficiently absorbed by combining an absorber, and the influence factors such as the concentration and the dosage of the absorption liquid, the PH of the liquid to be detected and the like are reduced by adopting a direct titration method, so that the precision is improved;
2. the test range is wider, the quantitative detection of the ammonia content in the fly ash within the range of 10ppm to 10000ppm can be realized, and the applicability is stronger; the operation is simple, and the measurement can be quickly realized (the time length of a single test is less than 20 min); the method has the advantages of few influencing factors, higher data accuracy (5 percent of relative standard deviation), and low test cost, thereby having extremely strong popularization and application values in the aspect of quick detection of the ammonia in the fly ash and other building material products.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below, and it is apparent that the drawings in the following description only relate to some embodiments of the present invention and are not limiting on the present invention.
FIG. 1 is a schematic diagram of the apparatus of the present invention;
FIG. 2 is a schematic cross-sectional view of the splash separator of the present invention;
FIG. 3 is a schematic view of the connection structure of the liquid accumulation bottle, the absorption liquid reagent bottle, the absorber and the absorption pipeline according to the present invention;
FIG. 4 is a schematic circuit diagram of a color recognition device according to the present invention;
shown in the drawings
1-a steam generating bottle, 2-an electric heating element, 3-a steam pipeline, 5-a distillation tube, 6-a sealing plug, 7-an alkali liquor reagent bottle, 8-an alkali liquor valve, 9-a sample chamber, 10-a sample adding valve and 11-an electronic liquid level meter;
21-a splash-proof water-vapor separator, 22-a reflux condenser pipe, 23-a dryer;
211-a front chamber, 212-a splash guard, 213-a reflux hole, 214-a heat preservation interlayer, 215-a steam inlet, 216-a rear chamber, 217-a steam outlet;
31-liquid accumulation bottle, 32-absorption liquid reagent bottle, 33-acid liquid valve, 34-absorber, 35-one-way valve, 36-absorption pipeline;
41-magnetic stirrer, 42-color recognition device, 43-flowmeter, 44-titration liquid reagent bottle;
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The use of the word "comprising" or "comprises", and the like, in this disclosure is intended to mean that the elements or items listed before that word, include the elements or items listed after that word, and their equivalents, without excluding other elements or items. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
The invention is further illustrated with reference to the following figures and examples.
As shown in fig. 1 to 4, a quantitative test device for ammonia nitrogen substances in fly ash comprises a distillation unit for generating steam, a distillation tube 5, a separation unit for separating ammonia gas, an absorption unit and a titration metering unit, wherein the distillation unit is connected with the distillation tube 5 and an anti-splash water-vapor separator 21 arranged at the upper end of the distillation tube 5 through a steam pipeline 3, one end of the separation unit is connected with the upper end of the anti-splash water-vapor separator 21, the other end of the separation unit is connected with the absorption unit, and the titration metering unit is used for titrating ammonia-containing liquid to be tested in the absorption unit;
the anti-splash water-vapor separator 21 comprises a front chamber 211 and a rear chamber 216, wherein an anti-splash disc 212 is arranged above the front chamber 211 and extends into the rear chamber 216, the edge of the anti-splash disc 212 is opened to serve as a passage of distilled gas, heat-insulating interlayers 214 are wrapped outside the front chamber 211 and the rear chamber 216, a steam inlet 215 and a steam outlet 217 are arranged on the heat-insulating interlayer 214, and a one-way valve is arranged on the steam outlet 217;
the splash-proof disc 212 and the front cavity 211 are of an integral structure, the splash-proof disc 212 can effectively prevent reaction liquid from boiling over and entering a subsequent pipeline, water vapor condensed on the splash-proof disc 212 flows back to the front cavity 211 through a backflow hole 213 formed between the front cavity 211 and the rear cavity 216 and then enters the distillation tube 5, the front cavity 211 is communicated with the inside of the distillation tube 5, a sealing plug 6 is arranged at the joint, distillation gas of the distillation tube 5 sequentially enters the front cavity 211 and the rear cavity 216, the rear cavity 216 is connected with the backflow condensation tube 22, and separated gas is output; hot steam is introduced into the heat-insulating interlayer 214 to increase the working temperature of the anti-splash steam separator 21, reduce the solubility of ammonia gas and improve the separation efficiency; the inclined reflux condensation pipe 22 is combined with the anti-splash water-vapor separator 21 to carry out reflux design, so that the effect of cooling reflux is achieved, the absorption efficiency is improved, and the effect of diluting the concentration of the liquid to be detected by condensed water vapor is reduced; the outlet of the reflux condensation pipe 22 is connected with a dryer 23, the dryer 23 is filled with an alkaline desiccant, ammonia and water vapor are further separated, and the influence of the water vapor is reduced.
The distillation unit comprises a steam generation bottle 1 and an electric heating element 2 arranged in the steam generation bottle 1, the electric heating element 2 is an electric heating pipe, the electric heating element 2 heats distilled water in the steam generation bottle 1 to generate hot steam, the hot steam enters a distillation pipe 5 and a splash-proof water-steam separator 21 through a steam pipeline 3 to perform steam stripping distillation and heating separation, and the extraction and separation efficiency of ammonia gas is improved;
an alkali liquor reagent bottle 7 and a sample chamber 9 which are communicated with the inside of the distillation tube 5 are arranged above the distillation tube 5, the alkali liquor reagent bottle 7 controls the adding amount of alkali liquor in the distillation tube 5 by opening and closing an alkali liquor valve 8 arranged on a pipeline between the alkali liquor reagent bottle 7 and the distillation tube 5, the sample chamber 9 soaks the fly ash sample, the fly ash sample is washed to enter the distillation tube 5, and a sample adding valve 10 arranged on the pipeline between the sample chamber 9 and the distillation tube 5 is closed to keep the sealing performance.
The separation unit comprises a reflux condenser pipe 22 obliquely arranged at the upper end of the splash-proof water-vapor separator 21 and a dryer 23 arranged at the right end of the reflux condenser pipe 22, the reflux condenser pipe 22 adopts an oblique reflux mode, an inlet is connected with the splash-proof water-vapor separator 21, an outlet is connected with the dryer 23 and used for reducing the temperature of the distilled gas to avoid introducing a large amount of water vapor into the absorption liquid, the dryer 23 is filled with quicklime to further separate ammonia and water vapor, and simultaneously, the water vapor is prevented from being introduced to greatly dilute the concentration of the ammonia-containing liquid to be detected; the dryer 23 is provided with a medicine replacement port and a discharge port, so that the drying agent can be replaced conveniently.
The absorption unit comprises a liquid accumulation bottle 31, an absorption liquid reagent bottle 32 and an absorption pipeline 36, one end of the absorption pipeline 36 is connected with the dryer 23, the other end of the absorption pipeline extends into the bottom of the liquid accumulation bottle 31, the bottom of the liquid accumulation bottle 31 is provided with a parallel lens, and the absorption liquid reagent bottle 32 is connected with the liquid accumulation bottle 31 through a pipeline.
As shown in fig. 2, two absorbers 34 are arranged on the absorption pipeline 36 to improve the absorption efficiency of ammonia gas; the two absorbers 34 are communicated through inclined pipelines and the upper end opening is sealed by a sealing plug, the first-stage absorber is connected with the absorption liquid reagent bottle 32 and is connected to the bottom of the second-stage absorber through a pipeline from the upper part of the first-stage absorber, the unabsorbed ammonia gas in the first-stage absorber enters the second-stage absorber through a communication pipeline for further absorption, and finally the absorption liquid is discharged into the liquid collecting bottle 31 below;
preferably, the absorption pipeline 36 is provided with a plurality of absorbers 34 to improve the absorption efficiency of the ammonia gas; when the absorption line 36 is provided with a plurality of absorbers 34, the absorption effect is better. A check valve 35 is provided on the absorption line 36 above the absorber 34 to prevent backflow into the absorber 34 or the dryer 23.
The titration metering unit comprises a magnetic stirrer 41 for stirring the liquid accumulation bottle 31, a color recognition device 42 for recognizing a color change judgment end point, a flow meter 43 and a titration liquid reagent bottle 44, wherein parallel lenses of light-permeable sources are arranged on two sides of the bottom of the liquid accumulation bottle 31, a light source enters from one side and enters from the other side into the color recognition device 42, and a reagent in the titration liquid reagent bottle 44 is pumped into the liquid accumulation bottle 31 through a pump and the consumption of the reagent is metered through the flow meter 43. The color recognition device 42 is a color recognition sensor module integrating a TCS34725 chip and an MCU (model MINIATMEGA328P-AU) chip, and is IIC or serial communication to directly output RGB values, and the working principle is that after a light source irradiates an object to be detected, the return light detects RGB ratio values through a filter, and recognizes colors according to the RGB ratio values, as shown in fig. 4.
The alkali liquor valve 8, the sample adding valve 10, the acid liquor valve 33 and other valves on the pipeline can be electromagnetic valves, and the automatic integrated controller controls the electromagnetic valves through a relay to realize the automatic opening and closing of the valves on the pipeline; the automatic integrated controller controls the opening and closing of the electric heating element 2 through a relay and controls the opening and closing of a valve on a water inlet pipe of the steam generating bottle 1 according to an electronic liquid level meter 11 arranged on the steam generating bottle 1; in the titration metering unit, an automatic integrated controller can control the opening and closing of the magnetic stirrer 41 through a relay, so that automatic stirring is realized. The automatic integrated controller may be a PLC controller, and includes a 16-bit or 32-bit MCU chip, a clock circuit, an amplifying circuit, a memory module, and the like (prior art, which is not described herein again).
A quantitative test method for ammonia nitrogen substances in fly ash comprises the following steps:
s1, cleaning by using ammonia-free distilled water, connecting the device, distilling and titrating a blank sample, and discharging residual ammonia gas in the device or reducing the influence of ammonia in the solution so as to improve the test precision and reduce the experiment interference;
weighing a certain mass of fly ash, filling the fly ash into a sample chamber 9, adding distilled water for soaking and flushing the fly ash into a distillation tube 5, and keeping the tightness of the device;
s2, under a sealed state, firstly, adding an absorption liquid into the liquid accumulation bottle 31, wherein the absorption liquid is boric acid with the mass concentration of 1.5-4 wt%, and the mass ratio of the absorption liquid to the fly ash sample is as follows: (20-200): 5-30);
then, adding 5-50 wt% of sodium hydroxide or potassium hydroxide serving as an alkaline reaction solution into the distillation tube 5 through an alkaline solution reagent bottle 7, wherein the mass ratio of the alkaline reaction solution to the fly ash sample is as follows: (5-50): (5-30);
opening the condensation circulating water of the reflux condensation pipe 22, introducing hot steam generated by the distillation unit into the bottom of the distillation pipe 5 and the anti-splash steam separator 21, accelerating the reaction in the distillation pipe 5 and realizing steam stripping distillation, and setting the distillation time;
s3, after splash-proof water-vapor separation, condensation reflux and drying treatment, introducing the distillate gas into an absorption unit to be absorbed by absorption liquid to obtain liquid containing ammonia to be detected;
s4, adding a color indicator into the ammonia-containing solution to be detected, starting the magnetic stirrer 41 to stir the ammonia-containing solution to be detected, and dropwise adding a titration reagent with known concentration to a color change end point;
the color indicator is a methyl red-methylene blue solution or a methyl red-bromophenol green mixed indicator, the titration reagent is a standard dilute hydrochloric acid or dilute sulfuric acid solution with known concentration, and the concentration range is 0.001-0.1 mol/L; the ammonia-containing solution to be detected is mainly ammonium borate and excessive boric acid solution, a target product is directly titrated by using strong acid such as dilute hydrochloric acid or dilute sulfuric acid, and the titration of the weak acid and weak base salt of ammonium borate is not influenced by the pH of the titrated product, the concentration and the dosage of the absorption solution, so that interference factors are reduced, and the data stability is improved.
S5, calculating the content of ammonia nitrogen substances in the fly ash according to the consumption of the titration reagent, wherein the calculation formula of the ammonia content in the fly ash is as follows:
in the formula, X is the ammonia content of the fly ash, ppm; v2 is the volume of hydrochloric acid standard solution consumed by the test sample, ml; v0 is the volume, ml, of hydrochloric acid standard solution consumed by the measurement of the blank sample; m is the mass of the fly ash sample, g; c is the concentration of the titrated hydrochloric acid standard solution, mol/L.
Example 1
The results of the tests were compared for different ammonia containing ranges using standard ammonium chloride solutions of known concentrations of 0.38% and 0.0038%, and are shown in table 1.
Specific implementation parameters:
standard 0.0038% NH4Cl solution used: the sample mass is 30g, NaOH (50 wt%) solution is 5g, boric acid (4 wt%) solution is 20g, and the concentration of a standard hydrochloric acid titration reagent is 0.001 mol/L;
standard 0.38% NH4Cl solution used: the sample mass is 5g, NaOH (5 wt%) solution is 50g, boric acid (1.5 wt%) solution is 200g, and the concentration of standard hydrochloric acid titration reagent is 0.1 mol/L;
the implementation effect of the device is analyzed by adopting the solution with high ammonia concentration and the solution with low ammonia concentration, the theoretical ammonia content range of the ammonium chloride solid is 29-32%, the measured ammonia content of the ammonia-containing solution to be measured is converted into the actually measured ammonia content value of the solid ammonium chloride compound in the test, and the actually measured ammonia content value is compared with the theoretical value. Each group was tested three times and averaged to reflect the degree of dispersion between the parallel groups as the Standard Deviation (SD) and the Relative Standard Deviation (RSD) measures the relative error between the measured and true values.
TABLE 1 test of the effectiveness of the device
The test result shows that: by adopting the conventional method A1B1, the measured ammonia content value is basically out of the theoretical ammonia content range, the data accuracy is poor, the numerical standard deviation is large, and the data fluctuation is large; the method of stripping A2B1 can improve the accuracy of data, the measured value of high-concentration ammonia content basically fluctuates in the theoretical ammonia content range, and for the sample with low concentration, the measured value of ammonia content has larger deviation with the theoretical value and the relative standard deviation is larger; by adopting the method of A2B2, the concentration fluctuation of the ammonia-containing solution to be tested is the minimum, the data accuracy is the strongest, the measured value of the ammonia content is fluctuated in the theoretical ammonia content range, the data fluctuation is the minimum, and the test effect is the best.
Example 2
The applicability and the accuracy of the device and the method for testing the fly ash are verified.
The denitration fly ash C is a test sample, a 0.038 wt% NH4Cl solution is a standard substance, and the calculation formula of the obtained standard recovery is as follows:
p ═ standard (standard sample measurement value-sample measurement value)/standard addition value × 100(85 to 120% as the target value of recovery rate)
Specific implementation parameters:
the mass of the sample is 10-20 g, and the mass is accurately measured;
50g of NaOH (20 wt%) solution and 50g of boric acid (2.5 wt%) solution;
the concentration of a standard hydrochloric acid titration reagent is 0.05mol/L, and the concentration is diluted according to the concentration of a test sample, the actual concentration of hydrochloric acid is calibrated, and the distillation time is 8 min.
TABLE 5 spiking recovery test
Through a standard addition recovery test, the ammonia content concentration and the ammonia content recovery rate are both in a target recovery range (85-120%), close to 100%, and the numerical value fluctuation is small, so that the method has high accuracy and can be accurately used for quantitative measurement and analysis of the ammonia content of the fly ash.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The quantitative test device for the ammonia nitrogen substances in the fly ash is characterized by comprising a distillation unit, a distillation pipe (5), a separation unit, an absorption unit and a titration metering unit, wherein the distillation unit is connected with the distillation pipe (5) and an anti-splash water-vapor separator (21) arranged at the upper end of the distillation pipe (5) through a pipeline, one end of the separation unit is connected with the upper end of the anti-splash water-vapor separator (21), the other end of the separation unit is connected with the absorption unit, and the absorption unit is arranged on the titration metering unit;
the splash-proof water-vapor separator (21) comprises a front chamber (211) and a rear chamber (216), a splash-proof disc (212) is arranged above the front chamber (211) and extends into the rear chamber (216) and is communicated with the rear chamber (216), a backflow hole (213) is formed between the front chamber (211) and the rear chamber (216), a heat-preservation interlayer (214) is wrapped outside the front chamber (211) and the rear chamber (216), and a steam inlet (215) and a steam outlet (217) are formed in the heat-preservation interlayer (214).
2. The quantitative testing device for ammonia nitrogen substances in fly ash according to claim 1, wherein the distillation unit comprises a steam generating bottle (1) and an electric heating element (2) arranged in the steam generating bottle (1), and the electric heating element (2) is an electric heating pipe.
3. The quantitative testing device for the ammonia nitrogen substance in the fly ash as claimed in claim 2, wherein the distillation tube (5) is provided with an alkali liquor reagent bottle (7) and a sample chamber (9) which are both communicated with the inside of the distillation tube (5).
4. The quantitative testing device for ammonia nitrogen in fly ash as claimed in claim 3, wherein the separation unit comprises a reflux condenser pipe (22) obliquely arranged at the upper end of the anti-splash water-vapor separator (21), and a dryer (23) arranged at the right end of the reflux condenser pipe (22).
5. The quantitative testing device for the ammonia nitrogen substance in the fly ash as claimed in claim 4, wherein the absorption unit comprises a liquid accumulation bottle (31), an absorption liquid reagent bottle (32) and an absorption pipeline (36), one end of the absorption pipeline (36) is connected with the dryer (23), the other end of the absorption pipeline extends into the bottom of the liquid accumulation bottle (31), the bottom of the liquid accumulation bottle (31) is provided with a parallel lens, and the absorption pipeline (36) is provided with at least one absorber (34); the absorption liquid reagent bottle (32) is connected with the liquid accumulation bottle (31) or the absorber (34) through a pipeline.
6. The quantitative testing device for the ammonia nitrogen substance in the fly ash as claimed in claim 5, wherein the titration metering unit comprises a magnetic stirrer (41) for stirring the liquid accumulation bottle (31), a color recognition device (42) for recognizing a color change judgment end point, a flow meter (43), and a titration liquid reagent bottle (44), wherein a reagent in the titration liquid reagent bottle (44) is pumped into the liquid accumulation bottle (31) through a pump, and the consumption of the reagent is metered through the flow meter (43).
7. The quantitative testing device for the ammonia nitrogen substance in the fly ash as claimed in claim 1, wherein the testing device further comprises an automatic integrated controller, and the automatic integrated controller is used for controlling the on-off of the electric heating element (2) and controlling the on-off of a valve on a pipeline through a relay and an electromagnetic valve.
8. A quantitative test method for a fly ash ammonia nitrogen substance, which utilizes the quantitative test device for the fly ash ammonia nitrogen substance in any one of claims 1 to 7, and is characterized by comprising the following steps:
s1, cleaning by using ammonia-free distilled water, connecting the device, weighing a certain mass of fly ash, filling the fly ash into a sample chamber (9), adding distilled water for soaking and washing, and introducing the fly ash into a distillation tube (5) to keep the tightness of the device;
s2, under a sealed state, firstly adding absorption liquid into the liquid accumulation bottle (31), then adding excessive alkaline reaction liquid into the distillation pipe (5) through an alkaline liquid reagent bottle (7), introducing hot steam generated by the distillation unit into the distillation pipe (5) and the anti-splash steam separator (21), and carrying out steam stripping distillation;
s3, after splash-proof water-vapor separation, condensation reflux and drying treatment, introducing the distillate gas into an absorption unit to be absorbed by absorption liquid to obtain liquid containing ammonia to be detected;
s4, adding a color indicator into the ammonia-containing solution to be detected, starting a magnetic stirrer (41) to stir, and dropwise adding a titration reagent with known concentration to a color-changing end point;
s5, calculating the content of ammonia nitrogen substances in the fly ash according to the consumption of the titration reagent, wherein the calculation formula of the ammonia content in the fly ash is as follows:
in the formula, X is the ammonia content of the fly ash, ppm; v2 is the volume of hydrochloric acid standard solution consumed by the test sample, ml; v0 is the volume, ml, of hydrochloric acid standard solution consumed by the measurement of the blank sample; m is the mass of the fly ash sample, g; c is the concentration of the titrated hydrochloric acid standard solution, mol/L.
9. The quantitative test method for the ammonia nitrogen substance in the fly ash according to claim 8, wherein the alkaline reaction solution is sodium hydroxide or potassium hydroxide, the mass concentration is 5-50 wt%, and the mass ratio of the alkaline reaction solution to the fly ash sample is as follows: (5-50): (5-30);
the absorption liquid is boric acid, the mass concentration is 1.5-4 wt%, and the mass ratio of the absorption liquid to the fly ash sample is as follows: (20 to 200) and (5 to 30).
10. The quantitative test method for ammonia nitrogen substances in fly ash according to claim 8, wherein the color indicator is a methyl red-methylene blue solution or a methyl red-bromophenol green mixed indicator, and the titration reagent is a dilute hydrochloric acid or dilute sulfuric acid solution with a concentration range of 0.001-0.1 mol/L.
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