CN103163245B - Method for detecting content of ammonia in fly ash of coal-fired boiler - Google Patents
Method for detecting content of ammonia in fly ash of coal-fired boiler Download PDFInfo
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- CN103163245B CN103163245B CN201310085120.1A CN201310085120A CN103163245B CN 103163245 B CN103163245 B CN 103163245B CN 201310085120 A CN201310085120 A CN 201310085120A CN 103163245 B CN103163245 B CN 103163245B
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 229
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title abstract description 32
- 239000010881 fly ash Substances 0.000 title abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000006228 supernatant Substances 0.000 claims abstract description 44
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000012360 testing method Methods 0.000 claims description 118
- 239000000428 dust Substances 0.000 claims description 83
- 239000000523 sample Substances 0.000 claims description 81
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 51
- 150000002500 ions Chemical class 0.000 claims description 45
- 238000004587 chromatography analysis Methods 0.000 claims description 40
- 239000012488 sample solution Substances 0.000 claims description 39
- 238000001514 detection method Methods 0.000 claims description 30
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 5
- 238000010829 isocratic elution Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 abstract description 10
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000004568 cement Substances 0.000 abstract description 3
- -1 ammonium ions Chemical class 0.000 abstract 3
- 239000012086 standard solution Substances 0.000 description 26
- 239000000243 solution Substances 0.000 description 22
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000003546 flue gas Substances 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 230000008569 process Effects 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003189 isokinetic effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for detecting the content of ammonia in fly ash of a coal-fired boiler. The method comprises the following steps of: preparing a sample to be tested of the fly ash of the coal-fired boiler; mixing the sample to be tested and water so as to obtain a solution of the sample to be tested, wherein the mass ratio of the sample to be tested to the water is 1:(10-100); adjusting the pH value of the solution of the sample to be tested to be 6.0-6.8, stirring and standing the solution so as to obtain supernatant liquid, and detecting ammonium ions in the supernatant liquid so as to obtain the concentration of the ammonium ions in the supernatant liquid; calculating to obtain the mass of the ammonia in the sample to be tested according to the concentration of the ammonium ions; and calculating to obtain the content of the ammonia in the fly ash of the coal-fired boiler according to the mass of the ammonia in the sample to be tested and the mass of the sample to be tested. According to the method, the water cement ratio and the pH value of the sample to be tested can be controlled so as to enable most and even all of the ammonia in the fly ash to be dissolved in water, the ammonia escape cannot generated, and thus the accurate results can be obtained.
Description
Technical field
The present invention relates to Flue Gas Denitrification Technologies on Coal-fired Boilers field, relate in particular to the detection method of ammonia content in a kind of coal-burning boiler flying dust.
Background technology
Along with the development of China's power industry, the discharge capacity of NOx grows with each passing day, well-known, and NOx pollutes can form acid rain, photo-chemical smog, destroys ecologic environment, and its impact more and more causes people's concern and attention.Along with the raising of China's emission standard, coal fired power generation unit substantially requires to install SCR (selective catalytic reduction) equipment for denitrifying flue gas and falls low NOx drainage.
The principle of SCR denitrating flue gas is: under catalyst action, spray into ammonia, by NO in flue gas
xbe catalysed and reduced into N
2and H
2o, because the ammonia spraying into and flue gas can not be accomplished even mixing of 100%, in some region of reactor, the content of ammonia can be greater than the NO in flue gas
xcontent, so just causes ammonia relative surplus, thereby forms the escaping of ammonia.The escaping of ammonia exerts an influence to unit safety stable operation meeting, and main cause is: the water vapour in flue gas, SO
3and the escaping of ammonia, can generate ammonium hydrogen sulfate under certain condition, ammonium hydrogen sulfate is a kind of very sticky corrosive substance under liquid state, can Benitration reactor and upstream device be resulted in blockage and be corroded.At the renewable Ljungstrom air heater of the many employings of Chinese large-sized coal fired power generation unit, boiler air feed is heated at present.In air preheater, low-temperature end, flue-gas temperature is lower than the initial generation temperature of ammonium hydrogen sulfate, ammonium hydrogen sulfate will generate on the heat transfer element surface of the middle low-temperature end of air preheater like this, thereby make air preheater produce fouling on heat exchange hardware, corrosion, finally cause air preheater to occur pressure drop rising, the phenomenons such as reduction of heat exchange efficiency, thereby cause induced draft fan running current to rise, boiler ventilation temperature reduces, thereby reduce the performance driving economy of unit, when air preheater stops up when serious, even can cause induced draft fan stall, thereby threaten the safe and stable operation of unit.Therefore, accurately monitor the escaping of ammonia of SCR flue gas denitrification system, for the escaping of ammonia of controlling denitrating system provides foundation, economy, safe operation to unit are most important.
The present invention studies and shows, the escaping of ammonia overwhelming majority being produced by denitrating system is adsorbed by flying dust, and is removed from flue gas by fly-ash separator together with flying dust.Therefore by the ammonia content in flying dust in periodic analysis fly-ash separator, can realize the monitoring to denitrating system the escaping of ammonia.But in prior art, there is no the standard of analyzing ammonia content in coal-burning boiler flying dust, the analysis and research of ammonia content in coal-burning boiler flying dust also be there is not yet to report.
Summary of the invention
The object of the present invention is to provide the detection method of ammonia content in a kind of coal-burning boiler flying dust, method provided by the invention can accurately obtain the ammonia content in coal-burning boiler flying dust, is conducive to industrial guidance.
The detection method that the invention provides ammonia content in a kind of coal-burning boiler flying dust, comprises the following steps:
The testing sample of coal-burning boiler flying dust is provided;
Described testing sample is mixed with water, obtain testing sample solution, the mass ratio of described testing sample and water is 1:(10～100);
Regulate pH value to 6.0～6.8 of described testing sample solution, after stirring, leaving standstill, the ammonium ion in the supernatant liquor obtaining is detected, obtain the concentration of ammonium ion in described supernatant liquor;
According to the concentration of described ammonium ion, calculate the quality of ammonia in testing sample;
According to the quality of ammonia in described testing sample and the quality of described testing sample, obtain the ammonia content in coal-burning boiler flying dust.
Preferably, described water is deionized water or pure water.
Preferably, the mass ratio of described testing sample and water is 1:(20～90).
Preferably, the mass ratio of described testing sample and water is 1:(30～80).
Preferably, pH value to 6.0～6.8 of the described testing sample solution of described adjusting are specially:
Described testing sample solution is mixed with acid compound, regulate pH value to 6.0～6.8 of described testing sample solution.
Preferably, the time of described stirring is 1 hour～3 hours.
Preferably, described the supernatant liquor obtaining is detected, obtains the concentration of ammonium ion in supernatant liquor and be specially:
The supernatant liquor obtaining is carried out to chromatography of ions detection, obtain the peak area of ammonium ion in supernatant liquor;
According to the peak area of ammonium ion in described supernatant liquor and predetermined NH
4 +concentration-peak area typical curve, obtain the concentration of ammonium ion in supernatant liquor.
The flow velocity of the leacheate that preferably, described chromatography of ions detects is 0.5mL/min～2mL/min.
Preferably, the type of elution that described chromatography of ions detects is isocratic elution;
The flow velocity of the leacheate that described chromatography of ions detects is 0.5mL/min～2mL/min.
Preferably, the column temperature that described chromatography of ions detects is 25 DEG C～35 DEG C;
The pond temperature that described chromatography of ions detects is 30 DEG C～40 DEG C;
The post that described chromatography of ions detects is pressed as 1000psi～1500psi.
The detection method that the invention provides ammonia content in a kind of coal-burning boiler flying dust, comprises the following steps: the testing sample that coal-burning boiler flying dust is provided; Described testing sample is mixed with water, obtain testing sample solution, the mass ratio of described testing sample and water is 1:(10～100); Regulate pH value to 6.0～6.8 of described testing sample solution, after stirring, leaving standstill, the ammonium ion in the supernatant liquor obtaining is detected, obtain the concentration of ammonium ion in described supernatant liquor; According to the concentration of described ammonium ion, calculate the quality of ammonia in testing sample; According to the quality of ammonia in described testing sample and the quality of described testing sample, obtain the ammonia content in coal-burning boiler flying dust.Method provided by the invention is mixed the testing sample of boiler fly ash with water, the water-soluble formation ammonium ion of ammonia wherein, the content that detects ammonium ion in solution can obtain the quality of ammonia, thereby obtains the ammonia content in testing sample according to the quality of the quality of ammonia and testing sample.Method provided by the invention is after mixing testing sample with water, the mass ratio that makes testing sample and water is (10～100): 1, and the pH value of controlling the solution to be measured obtaining is 6.0～6.8, thereby can make ammonia in testing sample can the overwhelming majority even all soluble in water, and can not there is the escape of ammonia, and the solution to be measured obtaining under condition is like this conducive to the wherein detection of ammonium ion content, thereby make method provided by the invention can obtain the ammonia content in flying dust more accurately.Experimental result shows, ammonia content and denitrating system the escaping of ammonia that method provided by the invention obtains in air preheater outlet flying dust are linear dependence relation, linearly dependent coefficient R
2be 0.909, this explanation, method provided by the invention can realize the accurate detection to the ammonia content in coal-burning boiler flying dust.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of embodiment of the present invention testing process.
Embodiment
The detection method that the invention provides ammonia content in a kind of coal-burning boiler flying dust, comprises the following steps:
The testing sample of coal-burning boiler flying dust is provided;
Described testing sample is mixed with water, obtain testing sample solution, the mass ratio of described testing sample and water is (10～100): 1;
Regulate pH value to 6.0～6.8 of described testing sample solution, after stirring, leaving standstill, will obtain supernatant liquor and detect, the concentration of ammonium ion in described supernatant liquor;
According to the concentration of described ammonium ion, calculate the quality of ammonia; According to the quality of the quality of described ammonia and described testing sample, obtain the ammonia content in coal-burning boiler flying dust.
The invention provides the detection method of ammonia content in a kind of boiler fly ash, flying dust sample to be measured is mixed with water, by controlling the water cement ratio in mixed process, the pH value of solution, make the ammonia overwhelming majority in flying dust even all soluble in water, and the supernatant obtaining is under these conditions easy to detect, and makes the testing result that obtains more accurate.Method provided by the invention has realized the Accurate Determining to ammonia content in boiler fly ash, is conducive to commercial production to instruct.
Although ammonia is very easily water-soluble, can, by by water-soluble the ammonia in flying dust, detect the content of ammonium ion in water, indirectly obtain ammonia content in flying dust.But the present invention's research shows, the control of the factor such as pH and stirring of water cement ratio, the sample solution that obtains can affect the mensuration to ammonia, in method provided by the invention, the mass ratio of flying dust testing sample and water is 1:(10～100), the pH value of controlling testing sample solution is 6.0～6.8, makes the testing result of the ammonia content obtaining accurate.
The invention provides the testing sample of coal-burning boiler flying dust.The present invention does not have special restriction to the source of described boiler fly ash, the flying dust that any process produces in coal-burning boiler can, as detected the flying dust of air preheater outlet.The present invention, for the testing result that makes to obtain is representative and authenticity, preferably samples the flying dust of same device different parts, then by even the flying dust sample mix obtaining, obtains the testing sample of flying dust.The present invention does not have special restriction to the mode of described sampling, adopts sampling mode well known to those skilled in the art, as the mode that can adopt isokinetic sampling is carried out Fly ash sampling.
Obtain after the testing sample of flying dust, the present invention mixes the testing sample of described flying dust with water, obtain testing sample solution, and the mass ratio of described testing sample and water is 1:(10～100).The present invention preferably gets sample segment and detects from the testing sample obtaining, and the sample segment of taking-up is weighed, and is preferably accurate to 0.0001g, and load weighted sample is placed in to beaker; Then to injected water in described beaker, obtain testing sample solution.In the present invention, described water is preferably one or both in deionized water or pure water, more preferably deionized water; The mass ratio of described testing sample and water is preferably 1:(20～90), more preferably 1:(30～80), most preferably be 1:(40～70) and, be the most preferably 1:50;
Obtain after testing sample solution, the present invention regulates pH value to 6.0～6.8 of described testing sample solution.The present invention preferably mixes described testing sample solution with acid compound, regulate pH value to 6.0～6.8 of described solution example to be measured.The present invention does not have special restriction to the kind of described acid compound, adopt the acid compound as pH value correctives well known to those skilled in the art, in the present invention, described acid compound is preferably hydrochloric acid or sulfuric acid, more preferably hydrochloric acid solution or sulfuric acid solution.The present invention does not have special restriction to the concentration of described hydrochloric acid solution or sulfuric acid solution, adopts sulfuric acid solution or the hydrochloric acid solution as pH value correctives well known to those skilled in the art.In the present invention, the mass concentration of described hydrochloric acid solution is preferably 1%～30%, and more preferably 5%～20%, most preferably be 10%～15%; The concentration of described sulfuric acid solution is preferably 1%～15%, and more preferably 3%～10%, most preferably be 5%～8%;
The present invention is in order to control more easily the pH value of testing sample solution, preferably adopt potentiometric titrimeter to control the pH value of testing sample solution, acid compound is placed in to potentiometric titrimeter, pH value is set between 6.0～6.8, the amount of the acid compound by potentiometric titrimeter control titration, makes the maintaining between 6.0～6.8 of pH value stabilization of testing sample solution.The present invention does not have special restriction to the source of described potentiometric titrimeter, adopts potentiometric titrimeter well known to those skilled in the art.
Complete after the adjusting of described pH to be measured, the testing sample solution that the present invention is 6.0～6.8 by the pH value obtaining stirs, and after leaving standstill, the ammonium ion in the supernatant liquor obtaining is detected, and obtains the concentration of ammonium ion in described supernatant.The present invention is not particularly limited the method for described stirring, adopts the technical scheme of stirring well known to those skilled in the art, as adopted hand operated mixing, also can adopt mechanical raking.In the present invention, the time of described stirring is preferably 1 hour～and 3 hours, more preferably 2 hours;
Complete after described stirring, the present invention, by the solution left standstill obtaining, detects the ammonium ion in the supernatant liquor obtaining, and obtains the concentration of ammonium ion in described supernatant liquor.The present invention does not have special restriction to the detection method of described ammonium ion, the technical scheme that adopts ammonium ion well known to those skilled in the art to detect;
The present invention preferably adopts the chromatography of ions to detect the ammonium ion in described supernatant, obtains the peak area of ammonium ion in supernatant liquor; According to the peak area of described supernatant liquor and predetermined NH
4 +concentration-peak area typical curve, obtain the concentration of ammonium ion in supernatant liquor.The present invention detects to described chromatography of ions the instrument adopting does not have special restriction, adopts ion chromatograph well known to those skilled in the art, wears peace ICS-3000 type ion chromatograph as adopted; In the present invention, the chromatographic column that described chromatography of ions detects is preferably cation separation post, and described chromatography of ions detects the rejector adopting and is preferably ASRS3004-mm kation autosynthesis rejector; The inhibition electric current that described chromatography of ions detects is preferably 50mA～65mA, more preferably 56mA; The volume of the quantitative ring that described chromatography of ions detects is preferably 10 μ L; The separating column that described chromatography of ions detects is preferably CS12A-4 × 250mm cation separation post; The type of elution that described chromatography of ions detects is preferably isocratic elution; The flow velocity of the leacheate that described chromatography of ions detects is preferably 0.5mL/min～2mL/min, more preferably 1.0mL/min; The present invention does not have special restriction to the kind of described leacheate, conventional leacheate while adopting chromatography of ions well known to those skilled in the art to detect ammonium ion; The column temperature that described chromatography of ions detects is preferably 25 DEG C～35 DEG C, more preferably 30 DEG C; The pond temperature that described chromatography of ions detects is preferably 30 DEG C～40 DEG C, more preferably 35 DEG C; The post that described chromatography of ions detects is pressed and is preferably 1000psi～1500psi, and more preferably 1100psi～1400psi, most preferably is 1200psi～1300psi;
Obtain after the peak area of ammonium ion in supernatant, the present invention is according to the peak area of ammonium ion in described supernatant and predetermined NH
4 +concentration-peak area typical curve, obtain the concentration of ammonium ion in supernatant liquor.In the present invention, described predetermined NH
4 +concentration-peak area typical curve preferably in accordance with the following methods obtain:
NH is provided
4 +the standard solution of series concentration;
To described NH
4 +the standard solution of series concentration carries out chromatography of ions detection, obtains the NH of each concentration
4 +the chromatography of ions figure of standard solution;
According to the described chromatography of ions figure NH corresponding with it
4 +the concentration of standard solution, obtains NH
4 +concentration-peak area typical curve.
The invention provides NH
4 +the standard solution of series concentration, the present invention does not have special restriction to the source of described standard solution, adopts NH well known to those skilled in the art
4 +standard solution, as bought NH
4 +standard solution, also can prepare voluntarily, the present invention does not have special restriction to the compound method of described standard solution, adopts the compound method of standard solution well known to those skilled in the art.For NH
4 +the commercial goods of standard solution, the present invention can be diluted to required concentration as required, detects.In the present invention, described NH
4 +the mass concentration of standard solution be preferably 0.1mg/L～15mg/L, more preferably 0.2mg/L～10mg/L, most preferably is 0.2mg/L, 1.0mg/L, 2.0mg/L, 4.0mg/L and 10.0mg/L.
Obtain NH
4 +after the standard solution of series concentration, the present invention is to described NH
4 +the standard solution of series concentration carries out chromatography of ions detection, obtains the NH of each concentration
4 +the chromatography of ions figure of standard solution.The present invention preferably adopts the above-mentioned technical scheme that ammonium ion in supernatant is detected to described NH
4 +the standard solution of series concentration carries out chromatography of ions detection, does not repeat them here.The present invention is in order to improve the accuracy of the typical curve obtaining, preferably to described NH
4 +the standard solution of series concentration carries out Parallel testing 2 times～5 times, more preferably 3 times, the corresponding peak area obtaining is added and, get its mean value;
Obtain the NH of each concentration
4 +after the chromatography of ions figure of standard solution, the present invention calculates the NH of each concentration
4 +the peak area of standard solution, the NH corresponding with it according to the peak area obtaining
4 +the concentration of standard solution, obtains NH
4 +concentration-peak area typical curve.The present invention preferably adopts least square fitting-peak area curve to calibrate.
Obtain NH
4 +after concentration-peak area typical curve, the peak area of ammonium ion and described NH in the supernatant that the present invention obtains according to technique scheme
4 +concentration-peak area typical curve, obtains the concentration of ammonium ion in described supernatant.
Obtain after the concentration of ammonium ion in supernatant, the present invention calculates the quality of ammonia in testing sample, and the present invention can calculate the quality of ammonia according to formula shown in formula (I):
Wherein, C
ammoniafor the ammonia content in flying dust, unit is mg/kg;
C
icfor NH in supernatant
4 +concentration, unit is mg/L;
V is testing sample solution volume, and unit is L;
M is the quality of testing sample, and unit is g;
17 is the relative molecular mass of ammonia;
18 is NH
4 +relative molecular mass.
Obtain after the quality of ammonia in testing sample, the present invention, according to the quality of ammonia in described testing sample and the quality of described testing sample, obtains the ammonia content in coal-burning boiler flying dust.The present invention is in order to obtain accurate testing result, and in the time that the quality of testing sample is weighed, degree of accuracy is preferably 0.0001g.
The detection method that the invention provides ammonia content in a kind of coal-burning boiler flying dust, comprises the following steps: the testing sample that coal-burning boiler flying dust is provided; Described testing sample is mixed with water, obtain testing sample solution, the mass ratio of described testing sample and water is 1:(10～100); Regulate pH value to 6.0～6.8 of described testing sample solution, after stirring, leaving standstill, the ammonium ion in the supernatant liquor obtaining is detected, obtain the concentration of ammonium ion in described supernatant liquor; According to the concentration of described ammonium ion, calculate the quality of ammonia in testing sample; According to the quality of ammonia in described testing sample and the quality of described testing sample, obtain the ammonia content in coal-burning boiler flying dust.Method provided by the invention is mixed the testing sample of boiler fly ash with water, the water-soluble formation ammonium ion of ammonia wherein, the content that detects ammonium ion in solution can obtain the quality of ammonia, thereby obtains the ammonia content in testing sample according to the quality of the quality of ammonia and testing sample.Method provided by the invention is after mixing testing sample with water, the mass ratio that makes testing sample and water is (10～100): 1, and the pH value of controlling the solution to be measured obtaining is 6.0～6.8, thereby can make ammonia in testing sample can the overwhelming majority even all soluble in water, and can not there is the escape of ammonia, and the solution to be measured obtaining under condition is like this conducive to the wherein detection of ammonium ion content, thereby make method provided by the invention can obtain the ammonia content in flying dust more accurately.Experimental result shows, ammonia content and denitrating system the escaping of ammonia that method provided by the invention obtains in air preheater outlet flying dust are linear dependence relation, linearly dependent coefficient R
2be 0.909, this explanation, method provided by the invention can realize the accurate detection to the ammonia content in coal-burning boiler flying dust.
In order to further illustrate the present invention, below in conjunction with embodiment, the detection method of ammonia content in coal-burning boiler flying dust provided by the invention is described in detail, but they can not be interpreted as to limiting the scope of the present invention.
Sample in following embodiment is that the air preheater outlet of Nei Mou 1000MW power plant of Zhejiang Province is extracted the flying dust sample in flue gas by isokinetic sampling; The ion chromatograph adopting is for wearing peace ICS-3000 type ion chromatograph; NH
4 +standard solution is SGB-YYA060021, and mass concentration is 20mg/L, and uncertainty is 2%; It is ASRS3004-mm kation autosynthesis rejector that chromatography of ions detects rejector.
Embodiment 1
By the NH purchasing
4 +standard solution dilution preparation obtains the standard solution that mass concentration is 0.2mg/L, 1.0mg/L, 2.0mg/L, 4.0mg/L and 10.0mg/L, by the NH of above-mentioned series concentration
4 +standard solution is placed in chromatography of ions and detects, the inhibition electric current that chromatography of ions detects is 59mA, it is 10 μ L that quantitative ring body amasss, separating column is CS12A-4 × 250mm cation separation post, type of elution is isocratic elution, and leacheate flow velocity is 1.0mL/min, and column temperature is 30 DEG C, Chi Wen is 35 DEG C, and post is pressed as 1200psi;
The standard solution Parallel testing of each concentration 3 times, obtains the corresponding peak area of each concentration standard solution, then calibrates with least square fitting concentration-peak area curve, obtains NH
4 +typical curve.
Embodiment 2
According to the flow process shown in Fig. 1, weigh 1.0000g flying dust testing sample, be placed in beaker, then add wherein 10g deionized water, obtain flying dust sample solution;
The hydrochloric acid solution that is 20% by massfraction is placed in potentiometric titrimeter, then with potentiometric titrimeter, the pH value of described flying dust sample solution is controlled between 6.0～6.8, sample solution is stirred simultaneously;
Stir after 2 hours, sample solution is left standstill, the pH value that continues titrator control solution in electricity consumption position in the process stirring is between 6.0～6.8;
Supernatant after leaving standstill is placed in to ion chromatograph to be detected, the inhibition electric current that chromatography of ions detects is 59mA, it is 10 μ L that quantitative ring body amasss, separating column is CS12A-4 × 250mm cation separation post, and type of elution is isocratic elution, and leacheate flow velocity is 1.0mL/min, column temperature is 30 DEG C, Chi Wen is 35 DEG C, and post is pressed as 1200psi, obtains the chromatography of ions peak area of supernatant;
The NH obtaining according to the chromatography of ions peak area of described supernatant and embodiment 1
4 +typical curve, obtain the mass concentration of ammonium ion in supernatant;
According to the computing formula shown in the mass concentration of ammonium ion and formula (I), obtain the ammonia content in flying dust, result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the present invention 2～8.
Embodiment 3
According to the technical scheme of embodiment 2, the ammonia content in flying dust is detected, different, the quality of the present embodiment flying dust testing sample is 2.0000g; The quality of deionized water is 100g; The pH value of flying dust sample solution is between 6.1～6.7; The time of stirring is 1.5 hours, obtains the ammonia content in flying dust, and result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the present invention 2～8.
Embodiment 4
According to the technical scheme of embodiment 2, the ammonia content in flying dust is detected, different is, in the present embodiment, the quality of flying dust testing sample is 3.0000g, add 300g pure water, the pH value of flying dust sample solution is between 6.2～6.8, and the time of stirring is 1 hour, obtains the ammonia content in flying dust, result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the present invention 2～8.
Embodiment 5
According to the technical scheme of embodiment 2, the ammonia content in flying dust is detected, different is, in the present embodiment, the quality of flying dust testing sample is 4.0000g, add 80g pure water, the pH value of flying dust sample solution is 6.0～6.5, and mixing time is 0.5 hour, obtains the ammonia content in flying dust, result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the present invention 2～8.
Embodiment 6
According to the technical scheme of embodiment 2, the ammonia content in flying dust is detected, different is, in the present embodiment, the quality of flying dust testing sample is 5.0000g, add 350g pure water, the pH value of flying dust sample solution is 6.2～6.6, and mixing time is 2 hours, obtains the ammonia content in flying dust, result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the present invention 2～8.
Embodiment 7
According to the technical scheme of embodiment 2, the ammonia content in flying dust is detected, different is, in the present embodiment, the quality of flying dust testing sample is 6.0000g, add 480g pure water, the pH value of flying dust sample solution is 6.0～6.6, and mixing time is 1.8 hours, obtains the ammonia content in flying dust, result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the present invention 2～8.
Embodiment 8
According to the technical scheme of embodiment 2, the ammonia content in flying dust is detected, different is, in the present embodiment, the quality of flying dust testing sample is 10.0000g, the quality of deionized water is 400g, mixing time is 1.5 hours, obtain the ammonia content in flying dust, result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the present invention 2～8.
The testing result that table 1 embodiment of the present invention 2～8 obtains
As can be seen from Table 1, in denitrating system the escaping of ammonia and air preheater outlet flying dust, ammonia content is all with the reducing and reduce of denitrating system, and ammonia content in denitrating system the escaping of ammonia and air preheater outlet flying dust is linear dependence relation, linearly dependent coefficient R
2be 0.909, this result conforms to actual conditions.Therefore can think the present invention be a kind of can be to carry out the analytical approach of Accurate Analysis containing the ammonia content in the coal-burning boiler flying dust of equipment for denitrifying flue gas.
As seen from the above embodiment, the invention provides the detection method of ammonia content in a kind of coal-burning boiler flying dust, comprise the following steps: the testing sample that coal-burning boiler flying dust is provided; Described testing sample is mixed with water, obtain testing sample solution, the mass ratio of described testing sample and water is (10～100): 1; Regulate pH value to 6.0～6.8 of described testing sample solution, after stirring, leaving standstill, will obtain supernatant liquor and detect, the concentration of ammonium ion in described supernatant liquor; According to the concentration of described ammonium ion, calculate the quality of ammonia; According to the quality of the quality of described ammonia and described testing sample, obtain the ammonia content in coal-burning boiler flying dust.Method provided by the invention is mixed the testing sample of boiler fly ash with water, the water-soluble formation ammonium ion of ammonia wherein, the content that detects ammonium ion in solution can obtain the quality of ammonia, thereby obtains the ammonia content in testing sample according to the quality of the quality of ammonia and testing sample.Method provided by the invention is after mixing testing sample with water, the mass ratio that makes testing sample and water is (10～100): 1, and the pH value of controlling the solution to be measured obtaining is 6.0～6.8, thereby can make ammonia in testing sample can the overwhelming majority even all soluble in water, and can not there is the escape of ammonia, and the solution to be measured obtaining under condition is like this conducive to the wherein detection of ammonium ion content, thereby make method provided by the invention can obtain the ammonia content in flying dust more accurately.Experimental result shows, ammonia content and denitrating system the escaping of ammonia that method provided by the invention obtains in air preheater outlet flying dust are linear dependence relation, linearly dependent coefficient R
2be 0.909, this explanation, method provided by the invention can realize the accurate detection to the ammonia content in coal-burning boiler flying dust.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a detection method for ammonia content in coal-burning boiler flying dust, comprises the following steps:
The testing sample of coal-burning boiler flying dust is provided;
Described testing sample is mixed with water, obtain testing sample solution, the mass ratio of described testing sample and water is 1:(20～90);
Regulate pH value to 6.0～6.8 of described testing sample solution, after stirring, leaving standstill, the ammonium ion in the supernatant liquor obtaining is carried out to chromatography of ions detection, obtain the peak area of ammonium ion in described supernatant liquor;
According to the peak area of ammonium ion in described supernatant liquor and predetermined NH
4 +concentration-peak area typical curve, obtain the concentration of ammonium ion in supernatant liquor;
According to the concentration of described ammonium ion, calculate the quality of ammonia in testing sample;
According to the quality of ammonia in described testing sample and the quality of described testing sample, obtain the ammonia content in coal-burning boiler flying dust.
2. detection method according to claim 1, is characterized in that, described water is deionized water or pure water.
3. according to the detection method described in claim 1～2 any one, it is characterized in that, the mass ratio of described testing sample and water is 1:(30～80).
4. detection method according to claim 1, is characterized in that, pH value to 6.0～6.8 of the described testing sample solution of described adjusting are specially:
Described testing sample solution is mixed with acid compound, regulate pH value to 6.0～6.8 of described testing sample solution.
5. detection method according to claim 1, is characterized in that, the time of described stirring is 1 hour～3 hours.
6. detection method according to claim 1, is characterized in that, the flow velocity of the leacheate that described chromatography of ions detects is 0.5mL/min～2mL/min.
7. detection method according to claim 1, is characterized in that, the type of elution that described chromatography of ions detects is isocratic elution;
The flow velocity of the leacheate that described chromatography of ions detects is 0.5mL/min～2mL/min.
8. detection method according to claim 1, is characterized in that, the column temperature that described chromatography of ions detects is 25 DEG C～35 DEG C;
The pond temperature that described chromatography of ions detects is 30 DEG C～40 DEG C;
The post that described chromatography of ions detects is pressed as 1000psi～1500psi.
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| CN103344594B (en) * | 2013-07-23 | 2016-05-11 | 河南省建筑科学研究院有限公司 | The detection method of ammonia burst size in flyash |
| CN106198860A (en) * | 2016-06-28 | 2016-12-07 | 盐城工学院 | A kind of method and system of the escaping of ammonia detection |
| CN107014946A (en) * | 2017-04-28 | 2017-08-04 | 国网天津市电力公司 | A kind of SCR denitration device ammonia consumption computational methods |
| CN108802234B (en) * | 2018-07-05 | 2021-05-07 | 科之杰新材料集团有限公司 | Method for measuring content of ammonium ions in fly ash |
| CN112526059A (en) * | 2020-10-23 | 2021-03-19 | 福建天辰耀隆新材料有限公司 | Method for determining and analyzing ammonia content in ammoximation reaction clear liquid |
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