CN103712981A - Method for detecting content of nitrogen in denitrified fly ash - Google Patents
Method for detecting content of nitrogen in denitrified fly ash Download PDFInfo
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- CN103712981A CN103712981A CN201310674839.9A CN201310674839A CN103712981A CN 103712981 A CN103712981 A CN 103712981A CN 201310674839 A CN201310674839 A CN 201310674839A CN 103712981 A CN103712981 A CN 103712981A
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Abstract
The invention discloses a method for detecting the content of nitrogen in denitrified fly ash. The method comprises the following steps: distilling ammonium nitrogen of denitrified fly ash in a strong alkaline solution, titrating by adopting a hydrochloric acid solution, and calculating to obtain the content of nitrogen in the denitrified fly ash. The method for detecting the content of nitrogen in denitrified fly ash is made against the new solid wastes like the denitrified fly ash with the specific existing form of nitrogen as a starting point, is rapid and sensitive, fills a gap in the above performance index detection method of the denitrified fly ash, and can be widely used for the performance evaluation and quality control of the denitrified fly ash by coal-fired power plants and third party detection mechanisms.
Description
Technical field
The invention belongs to building materials detection technique field, be specifically related to a kind of denitration flyash nitrogen content detection method.
Background technology
Atmospheric pollution is serious, NO
xreducing discharging and become power industry development common recognition, is the important content of China " 12 " work.During the plans " 12 " such as < < energy-saving and emission-reduction " 12 " planning > > (No. (2012) 40, promulgated by the State Council), the comprehensive programme of work > of < < " 12 " energy-saving and emission-reduction > (No. (2011) 26, promulgated by the State Council) " completing the coal-fired unit denitration of 400,000,000 kilowatts of active services Facilities Construction; to the technological transformation of 70,000,000 kilowatts of coal-fired units low nitrogen burnings, denitration efficiency reaches more than 75% ".Expection " power industry nitrogen oxide emission in 2015 is reduced to 7,500,000 tons, the range of decrease 29% ".The denitration work of whole nation power industry is carried out just on a large scale.
Compulsory execution along with electric power denitration, tradition flyash will all become denitration flyash, affected by denitrating technique, denitrfying agent (urea, ammonia etc.), denitration product are overflowed endless, in residual flyash, can cause in flyash the chemical composition such as ammonium salt higher, and then the disposal of denitration flyash and comprehensive utilization are brought to adverse influence.But at present domesticly not yet denitration flyash is carried out to systematic study; context of detection at denitration flyash nitrogen element; in existing detection mode, elemental analyser sensitivity is not high; Kjeldahl's methods etc. are comparatively loaded down with trivial details; the demand of the large-scale promotion application of denitration flyash and safety guarantee be can not meet well, detection method and the respective standard of setting up scientific and effective denitration flyash nitrogen content needed badly.
Summary of the invention
The object of this invention is to provide a kind of denitration flyash nitrogen content detection method, can the convenient content that effectively detects nitrogen in denitration flyash.
Technical scheme of the present invention is:
A denitration flyash nitrogen content detection method, comprises the following steps:
(1) weighing quality is the natural drying denitration flyash of 1g, is accurate to 0.001g;
(2) build the distilling apparatus being formed by steam generator, reaction chamber and condenser pipe three parts;
(3) in conical flask, add 20mL boric acid absorption liquid, and drip 2 methyl red-bromcresol green indicator, the condenser pipe end of distilling apparatus is deep into and absorbs the following 1cm of liquid level place, then step (1) is claimed flyash pack into distillation generator in, add 10mL sodium hydroxide solution, start steam generator and carry out steam distillation, while being neutral to distillate, distillation finishes, with boric acid absorption liquid washing condenser pipe end;
(4) with hydrochloric acid standard solution titration distillate, solution records the accurate liquor capacity V1 of used salt acidity scale when green becomes lavender, and described hydrochloric acid standard solution concentration is c0=0.02mol/L, with natrium carbonicum calcinatum, demarcates;
(5) synchronize and carry out blank assay with flyash sample mensuration, except not adding all the other operation stepss sample, all with the mensuration of sample, record the accurate liquor capacity V2 of used salt acidity scale; Described blank assay consumes hydrochloric acid standard solution volume generally should not surpass 0.1mL;
(6) nitrogen content c(%) by formula I, calculate:
Acquired results is accurate to 0.01%.
Addend grain beaded glass in steam generator in step (2), checks after impermeability, with distilled water, carries out blank distillation, and by the distillate of water, pipeline is cleaned.
Described in step (3), methyl red-bromcresol green indicator, for taking 0.3g bromcresol green and 0.2g methyl red, is dissolved in the ethanol of 100mL95% volumetric concentration completely.
Described in step (3), boric acid absorption liquid concentration is 2%, the m/V of unit.
Described in step (3), concentration of sodium hydroxide solution is 40%, the m/V of unit.
By the investigation of coal-burning power plant's denitrating technique and the analysis of denitration flyash nitrogen content existence form are shown, in denitration flyash, nitrogen is mainly adsorbed in fly ash grain surface with ammonia state, different from the detection method of organic nitrogen, this method, without clearing up step, has been simplified experiment flow greatly.
Accompanying drawing explanation
Fig. 1 is the scheme of installation of the distilling apparatus of the nitrogen that uses of the present invention, 1. electric furnace, 2. steam generator, 3. bursting tube, 4. proofed sleeve, 5. alkali lye chamber, 6. reaction chamber, 7. adding mouth, 8. bursting tube, 9. condenser pipe, 10. receiving flask, 11. bar-shaped glass plugs, 12. clips.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment be take technical solution of the present invention and is implemented under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
1, in Shanghai City, 4 kinds of denitration flyash samples are got by different coal-burning power plants, weigh respectively the natural drying lower denitration flyash sample of 1.000g.
2, reagent is prepared:
Methyl red-bromcresol green indicator: take 0.3g bromcresol green and 0.2g methyl red, be dissolved in completely in 100mL95% volumetric concentration ethanol;
2% boric acid absorption liquid: take 2g boric acid and be dissolved in 1L deionized water;
40% sodium hydroxide solution: take 40g dissolution of sodium hydroxide in 1L deionized water;
0.02mol/L salt standard acid solution: the hydrochloric acid 16.7mL that draws ρ=1.19g/mL is dissolved in 100mL volumetric flask, and shake up to scale with distilled water diluting, draw this solution 10.0mL in 1000mL volumetric flask, with distilled water diluting, to scale, shake up, then with natrium carbonicum calcinatum, demarcate.
Demarcate: accurately take the natrium carbonicum calcinatum 0.020g that had been dried in conical flask, add 25mL newly to boil and cooling distilled water and 2 indicator, with 0.20mol/L hydrochloric acid standard solution, be titrated to solution and become lavender from green, record consumes the volume V3 of hydrochloric acid standard solution, do blank assay simultaneously, record consumes the volume V4 of hydrochloric acid standard solution, calculates the concentration of hydrochloric acid standard solution by formula II, and calibration result need be got its mean value with double test portion.
3, by shown in Fig. 1, build distilling apparatus, complete impermeability and detect and clean.
4,4 class denitration flyash samples carry out distillation procedure successively, in conical flask, add 20mL boric acid absorption liquid, and drip 2 methyl red-bromcresol green indicator, the condenser pipe end of distilling apparatus is deep into and absorbs the following 1cm of liquid level place, then flyash sample is packed in distillation generator, slowly add 10mL sodium hydroxide solution, start steam generator and carry out steam distillation, during the about 50mL of distillate volume, with pH test paper, survey when distillate is neutrality and distill and finish, with a small amount of boric acid absorption liquid washing condenser pipe end.
5, with hydrochloric acid standard solution titration 4 class denitration flyash sample distillates, solution records the accurate liquor capacity V1 of used salt acidity scale when green becomes lavender.
6, synchronize with sample determination and carry out blank assay, except not adding all the other operation stepss sample, all with the mensuration of sample, record the accurate liquor capacity V2 of used salt acidity scale.
7, by formula I, calculate all kinds of denitration flyash nitrogen contents, the results are shown in Table 1, and contrast with Kjeldahl's method testing result.
Table 1 denitration flyash nitrogen content detects
As seen from table, the testing result of this method and Kjeldahl's method is very approaching, shows that this method is reliable, and more convenient.
Claims (5)
1. a denitration flyash nitrogen content detection method, is characterized in that, comprises the following steps:
(1) weighing quality is the natural drying denitration flyash of 1g, is accurate to 0.001g;
(2) build the distilling apparatus being formed by steam generator, reaction chamber and condenser pipe three parts;
(3) in conical flask, add 20mL boric acid absorption liquid, and drip 2 methyl red-bromcresol green indicator, the condenser pipe end of distilling apparatus is deep into and absorbs the following 1cm of liquid level place, then step (1) is claimed flyash pack into distillation generator in, add 10mL sodium hydroxide solution, start steam generator and carry out steam distillation, while being neutral to distillate, distillation finishes, with boric acid absorption liquid washing condenser pipe end;
(4) with hydrochloric acid standard solution titration distillate, solution records the accurate liquor capacity V1 of used salt acidity scale when green becomes lavender, and described hydrochloric acid standard solution concentration is c0=0.02mol/L, with natrium carbonicum calcinatum, demarcates;
(5) synchronize and carry out blank assay with flyash sample mensuration, except not adding all the other operation stepss sample, all with the mensuration of sample, record the accurate liquor capacity V2 of used salt acidity scale; Described blank assay consumes hydrochloric acid standard solution volume generally should not surpass 0.1mL;
(6) nitrogen content c(%) by formula I, calculate:
Acquired results is accurate to 0.01%.
2. denitration flyash nitrogen content detection method according to claim 1, is characterized in that, addend grain beaded glass in the steam generator in step (2) checks after impermeability, with distilled water, carries out blank distillation, and by the distillate of water, pipeline is cleaned.
3. denitration flyash nitrogen content detection method according to claim 1, it is characterized in that, described in step (3), methyl red-bromcresol green indicator, for taking 0.3g bromcresol green and 0.2g methyl red, is dissolved in the ethanol of 100mL95% volumetric concentration completely.
4. denitration flyash nitrogen content detection method according to claim 1, is characterized in that, described in step (3), boric acid absorption liquid concentration is 2%, the m/V of unit.
5. denitration flyash nitrogen content detection method according to claim 1, is characterized in that, described in step (3), concentration of sodium hydroxide solution is 40%, the m/V of unit.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082737A (en) * | 2016-06-22 | 2016-11-09 | 济南大学 | A kind of method of the simply modified denitration flyash of technique |
| CN106680054A (en) * | 2017-02-14 | 2017-05-17 | 深圳市能源环保有限公司 | Waste incineration fly ash chelate leach liquor and preparation and application method thereof |
| CN107300601A (en) * | 2017-08-08 | 2017-10-27 | 盐城工学院 | A kind of assay method of flyash ammonium ion content |
| CN108508135A (en) * | 2017-02-27 | 2018-09-07 | 北新集团建材股份有限公司 | The quantitative analysis method of ammonium ion in a kind of denitrating flue gas desulfurated plaster |
| CN109060693A (en) * | 2018-09-30 | 2018-12-21 | 天津市贰拾壹站检测技术有限公司 | The detection method of ammonia content in a kind of flyash |
| CN111751363A (en) * | 2020-06-19 | 2020-10-09 | 中建西部建设建材科学研究院有限公司 | Quantitative testing device and testing method for ammonia nitrogen substances in fly ash |
| CN111751362A (en) * | 2020-06-19 | 2020-10-09 | 中建西部建设建材科学研究院有限公司 | Testing device and method for rapidly judging ammonia content of fly ash |
| CN111751361A (en) * | 2020-06-19 | 2020-10-09 | 中建西部建设建材科学研究院有限公司 | Device and method for extracting and testing ammonia nitrogen substances in fly ash |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082737A (en) * | 2016-06-22 | 2016-11-09 | 济南大学 | A kind of method of the simply modified denitration flyash of technique |
| CN106680054A (en) * | 2017-02-14 | 2017-05-17 | 深圳市能源环保有限公司 | Waste incineration fly ash chelate leach liquor and preparation and application method thereof |
| CN108508135A (en) * | 2017-02-27 | 2018-09-07 | 北新集团建材股份有限公司 | The quantitative analysis method of ammonium ion in a kind of denitrating flue gas desulfurated plaster |
| CN107300601A (en) * | 2017-08-08 | 2017-10-27 | 盐城工学院 | A kind of assay method of flyash ammonium ion content |
| CN109060693A (en) * | 2018-09-30 | 2018-12-21 | 天津市贰拾壹站检测技术有限公司 | The detection method of ammonia content in a kind of flyash |
| CN111751363A (en) * | 2020-06-19 | 2020-10-09 | 中建西部建设建材科学研究院有限公司 | Quantitative testing device and testing method for ammonia nitrogen substances in fly ash |
| CN111751362A (en) * | 2020-06-19 | 2020-10-09 | 中建西部建设建材科学研究院有限公司 | Testing device and method for rapidly judging ammonia content of fly ash |
| CN111751361A (en) * | 2020-06-19 | 2020-10-09 | 中建西部建设建材科学研究院有限公司 | Device and method for extracting and testing ammonia nitrogen substances in fly ash |
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Application publication date: 20140409 |