CN116539659A - Method for measuring nitrogen content in carbon-containing dust - Google Patents
Method for measuring nitrogen content in carbon-containing dust Download PDFInfo
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- CN116539659A CN116539659A CN202310323878.8A CN202310323878A CN116539659A CN 116539659 A CN116539659 A CN 116539659A CN 202310323878 A CN202310323878 A CN 202310323878A CN 116539659 A CN116539659 A CN 116539659A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000000428 dust Substances 0.000 title claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 34
- 239000003245 coal Substances 0.000 claims abstract description 22
- 238000004458 analytical method Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- 230000009467 reduction Effects 0.000 claims abstract description 9
- 239000001307 helium Substances 0.000 claims abstract description 8
- 229910052734 helium Inorganic materials 0.000 claims abstract description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002485 combustion reaction Methods 0.000 claims abstract description 7
- 238000012937 correction Methods 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000012795 verification Methods 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 60
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 21
- 239000004215 Carbon black (E152) Substances 0.000 claims description 11
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 11
- 229930195733 hydrocarbon Natural products 0.000 claims description 11
- 150000002430 hydrocarbons Chemical class 0.000 claims description 11
- 238000005259 measurement Methods 0.000 claims description 6
- 239000002802 bituminous coal Substances 0.000 claims description 3
- 239000013068 control sample Substances 0.000 claims description 3
- 238000005502 peroxidation Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 2
- 150000002978 peroxides Chemical class 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 238000005245 sintering Methods 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000007696 Kjeldahl method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/18—Investigating or analyzing materials by the use of thermal means by investigating thermal conductivity
-
- 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
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring nitrogen content in carbon-containing dust, which comprises the following steps: s1, weighing a carbon-containing dust-removing sample and a coal standard sample according to a certain proportion, and controlling the total weight of a single mixed sample to be 95-105 mg; s2, fully mixing a carbon-containing dust-removing ash sample with a standard coal sample, and performing peroxide combustion in a high-temperature furnace after mixing; s3, filtering the combusted gas, collecting the filtered gas in a gas collecting bottle, fully and uniformly mixing the gas and the gas, and then entering CO 2 And H 2 An O infrared cell and a quantitative ring; s4, carrying the gas in the quantitative ring by helium gas and removing oxygen by a reduction furnace; s5, calculating the percentage of nitrogen content through heat conductivity change; s6, establishing a standard working curve; s7, carrying out 2-3 standard sample analyses along with the sample, and carrying out drift correction and verification on the instrument; s8, measuring and obtaining the nitrogen content in the sample. The method has the advantages of simple operation, high test speed and high accuracy of analysis results, and can meet the detection requirement of rapid analysisAnd (5) solving.
Description
Technical Field
The invention belongs to the technical field of steel smelting, and particularly relates to a method for measuring nitrogen content in carbon-containing dust.
Background
Dust, smoke dust and sludge generated in the steel smelting production process have high utilization value. The full utilization of various kinds of dust in iron and steel enterprises is an indispensable component in the production of modern iron and steel enterprises from the standpoint of reasonable utilization of resources or environmental protection and dust pollution elimination. The dust produced in the iron and steel smelting process has high iron content and can be recycled as sintering raw material. The nitrogen oxides NOx in the flue gas generated in the sintering process has the characteristics of large emission, large temperature fluctuation, high dust content, corrosiveness, toxic gas, unstable emission and the like, so that the formation of the nitrogen oxides NOx in the sintering process must be monitored and treated to reduce the pollution of the emission of the nitrogen oxides to the environment. The combined production practice shows that the formation of nitrogen oxides NOx during sintering is largely influenced by the N content in the sintering raw material. The most influencing raw fuel for sintering is pulverized coal, and then is coke powder, dust-removing ash and iron fine powder. Therefore, the accurate measurement of the nitrogen content in the dust-removing ash has very important significance for sintering smelting process and sintering flue gas denitration.
Because of the various types of the dust, the fluctuation of the carbon content is large, the production of each process is focused on different characteristics, but the measurement of the nitrogen element content in the dust is not reported at present. At present, the method for measuring the nitrogen content in the coal and the coke is a Kjeldahl method, but the Kjeldahl method has complicated analysis steps and long analysis time and is not easy to be mastered by operators. The invention adopts a thermal conductivity method to measure the nitrogen content in the dedusting ash.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a method for measuring the nitrogen content in carbon-containing dust.
The invention discloses a method for measuring the nitrogen content in carbon-containing dust, which comprises the following steps:
s1, weighing a carbon-containing dust-removing sample and a coal standard sample according to a certain proportion, and controlling the total weight of a single mixed sample to be 95-105 mg; then putting the mixture into a tin foil cup, and then extruding the tin foil cup into a water drop shape; sequentially placing the split-packed tin foil cups in a movable sample tray, wherein a plurality of blank analysis control sample placing holes are reserved on the movable sample tray, and samples are sequentially placed in the rest sample placing holes;
s2, fully mixing a carbon-containing dust-removing ash sample with a standard coal sample, and performing peroxidation combustion in a high-temperature furnace after mixing, wherein the oxygen purity is more than 99.5%, and the oxygen supply pressure is 0.18+/-0.01 MPa;
s3, filtering the combusted gas, collecting the filtered gas in a gas collecting bottle, fully and uniformly mixing the gas and the gas, and then entering CO 2 And H 2 An O infrared cell and a quantitative ring;
s4, carrying the gas in the quantitative ring by helium gas, removing oxygen by a reduction furnace and converting nitrogen oxides into N 2 The method comprises the steps of carrying out a first treatment on the surface of the The furnace temperature of the reduction furnace is controlled to be 700+/-5 ℃;
s5, detecting nitrogen through a hydrocarbon nitrogen element analyzer, and obtaining the percentage of helium content through detection;
s6, establishing a standard working curve: 5 bituminous coal standard samples with high, medium and low nitrogen content are selected and analyzed according to the steps to generate a correction curve; the nitrogen curve is a linear type, and the linear correlation coefficient R is more than 0.9990 and is the optimal linear type;
s7, carrying out 2-3 standard sample analyses along with the sample, and carrying out drift correction and verification on the instrument.
S8, calculating a result: to obtain the nitrogen content in the sample
According to the weighing proportion of the sample and the coal standard sample, the nitrogen content in the sample is calculated according to the following formula.
W (N measurement): instrument-measured nitrogen content in the sample
m: total sample weight, mg
W (N standard): nitrogen content of the added coal standard sample
50: weigh the coal standard sample, mg.
Preferably, the combustion-supporting gas of the hydrocarbon nitrogen element analyzer: oxygen with purity >99.5% and pressure (0.18+ -0.01) MPa; motive gas of hydrocarbon nitrogen analyzer: drying compressed air, wherein the pressure (0.18+/-0.01) MPa; the protective gas of the hydrocarbon nitrogen analyzer is helium with purity of 99.99 percent and pressure (0.18+/-0.01) MPa.
Preferably, the combustion temperature in the high temperature furnace is controlled to 950+/-5 ℃.
Preferably, the temperature of the reduction furnace is controlled at 700 ℃ + -5 ℃.
The invention has the advantages and technical effects that: the method is simple to operate, high in test speed and high in analysis result accuracy, and can meet the detection requirement of rapid analysis.
Drawings
Fig. 1 is a graph of nitrogen element detection operation.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides a method for measuring the nitrogen content in dust ash by adopting a thermal conductivity method, in particular to a method for measuring the nitrogen content in carbon-containing dust ash, which comprises the following steps:
s1, weighing a carbon-containing dust-removing sample and a coal standard sample according to a certain proportion, and controlling the total weight of a single mixed sample to be 95-105 mg; then putting the mixture into a tin foil cup, and then extruding the tin foil cup into a water drop shape, so that on one hand, the sample can smoothly enter the instrument, the sample clamping condition is avoided, and on the other hand, the air in the tin foil cup can be exhausted; sequentially placing the split-packed tin foil cups in a movable sample tray, wherein a plurality of blank analysis control sample prevention holes are reserved on the movable sample tray, and samples are sequentially placed in the rest sample placement holes;
s2, fully mixing a carbon-containing dust-removing ash sample with a standard coal sample, and performing peroxidation combustion in a high-temperature furnace after mixing, wherein the oxygen purity is more than 99.5%, and the oxygen supply pressure is 0.18+/-0.01 MPa;
s3, filtering the combusted gas, collecting the filtered gas in a gas collecting bottle, fully and uniformly mixing the gas and the gas, and then entering CO 2 And H 2 An O infrared cell and a quantitative ring;
s4, carrying the gas in the quantitative ring by helium gas, removing oxygen by a reduction furnace and converting nitrogen oxides into N 2 ；
S5, detecting nitrogen through a hydrocarbon nitrogen element analyzer, and calculating nitrogen content through the change of thermal conductivity of carrier gas;
s6, establishing a standard working curve: 5 bituminous coal standard samples with high, medium and low nitrogen content are selected and analyzed according to the steps to generate a correction curve; the nitrogen curve is a linear type, and the linear correlation coefficient R is more than 0.9990 and is the optimal linear type (refer to FIG. 1);
s7, carrying out 2-3 standard sample analyses along with the sample, and carrying out drift correction and verification on the instrument;
s8, calculating a result:
according to the weighing proportion of the sample and the coal standard sample, the nitrogen content in the sample is calculated according to the following formula.
W (N measurement): instrument-measured nitrogen content in the sample
m: total sample weight, mg
W (N standard): nitrogen content of the added coal standard sample
50: weigh the coal standard sample, mg.
The hydrocarbon nitrogen element analyzer is selected from: SDCHN435 hydrocarbon nitrogen analyzer (lakenan san de), combustion-supporting gas: oxygen with purity >99.5% and pressure (0.18+ -0.01) MPa. Power flow: the compressed air is dried and the pressure (0.18+/-0.01) MPa. Helium with purity >99.99% and pressure (0.18+ -0.01) MPa.
The used reagent comprises a tin foil cup and quartz wool; furnace reagents; copper wire; linear copper; alkali asbestos; magnesium perchlorate, nitrogen catalyst. The experimental instrument needs to be preheated for more than 3 hours in advance.
Preferably, the combustion temperature in the high temperature furnace is controlled to 950+/-5 ℃.
Preferably, the temperature of the reduction furnace is controlled at 700 ℃ + -5 ℃.
Control test: the nitrogen content of a 100mg dust-removing ash sample is directly measured, and experiments show that the sample burns incompletely and the experimental result is low.
The method comprises the following steps:
random test: randomly selecting three dedusting ash samples in the production process, mixing the dedusting ash samples with GBW11110 (N percent 1.00) standard coal according to different proportions, controlling the total weight within 95 mg-105 mg, analyzing, and obtaining the results shown in the table 1, wherein the test results are shown in the table 1, and the standard coal ratio experiment is shown in the table 1
Experiments show that the sample can be fully combusted by mixing 50mg of the dedusting ash sample and 50mg of the standard coal, the stability of the measurement result is better, and meanwhile, the calculation of the result is convenient.
Precision experiment: according to the experimental method, 3 dust samples are measured, a precision test is carried out, and the result of calculating the nitrogen content is shown in Table 2.
Table 2 results of precision test (n=11)
As can be seen from the data in the table, the RSD of all 3 samples is less than 3%, which indicates that the method has better precision.
The accuracy of the invention is verified: according to the method, 2 dust-removing ash samples are selected and respectively mixed with 3 standard coals (N percent: 0.69, 0.98 and 1.16) according to the proportion of 50mg (standard coals) +50mg (samples), and recovery tests are carried out, and the results are shown in Table 3
TABLE 3 labeling recovery test results
The data in the table shows that the recovery rate is 97.5% -102.1%, which shows that the method has higher accuracy.
In conclusion, the measuring method is simple to operate, high in testing speed and high in accuracy of analysis results, and can meet the detection requirement of rapid analysis.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (4)
1. A method for measuring the nitrogen content in carbon-containing dust ash is characterized by comprising the following steps: the method comprises the following steps:
s1, weighing a carbon-containing dust-removing sample and a coal standard sample according to a certain proportion, and controlling the total weight of a single mixed sample to be 95-105 mg; then placing the mixed sample into a tin foil cup, and extruding the tin foil cup into a water drop shape; sequentially placing the split-packed tin foil cups in a movable sample tray, wherein a plurality of blank analysis control sample placing holes are reserved on the movable sample tray, and samples are sequentially placed in the rest sample placing holes;
s2, fully mixing a carbon-containing dust-removing ash sample with a standard coal sample, and performing peroxidation combustion in a high-temperature furnace after mixing, wherein the oxygen purity is more than 99.5%, and the oxygen supply pressure is 0.18+/-0.01 MPa;
s3, filtering the combusted gas, collecting the filtered gas in a gas collecting bottle, fully and uniformly mixing the gas and the gas, and then entering CO 2 And H 2 An O infrared cell and a quantitative ring;
s4, removing the gas in the quantitative ring by carrying the helium gas through a reduction furnaceRemoving oxygen and converting nitrogen oxides to N 2 The method comprises the steps of carrying out a first treatment on the surface of the The furnace temperature of the reduction furnace is controlled to be 700+/-5 ℃;
s5, detecting nitrogen through a hydrocarbon nitrogen element analyzer, and determining the percentage of the nitrogen element content through the thermal conductivity measured by a thermal conductivity detector;
s6, establishing a standard working curve: 5 bituminous coal standard samples with high, medium and low nitrogen content are selected and analyzed according to the steps to generate a correction curve; the nitrogen curve is a linear type, and the linear correlation coefficient R is more than 0.9990 and is the optimal linear type;
s7, carrying out 2-3 standard sample analyses along with the sample, and carrying out drift correction and verification on the instrument.
S8, calculating a result: the nitrogen content in the sample was obtained.
According to the weighing proportion of the sample and the coal standard sample, calculating the nitrogen content in the sample according to the following formula;
w (N measurement): nitrogen content in the sample measured by the instrument;
m: total sample weight, mg;
w (N standard): adding the nitrogen content of the coal standard sample;
50: weigh the coal standard sample, mg.
2. The method for measuring the nitrogen content in the carbon-containing dust according to claim 1, wherein the method comprises the steps of:
combustion-supporting gas of hydrocarbon nitrogen element analyzer: oxygen with purity >99.5% and pressure (0.18+ -0.01) MPa;
motive gas of hydrocarbon nitrogen analyzer: drying compressed air, wherein the pressure (0.18+/-0.01) MPa;
the carrier gas of the hydrocarbon nitrogen analyzer is helium with purity of 99.99 percent and pressure (0.18+/-0.01) MPa.
3. The method for measuring the nitrogen content in the carbon-containing dust according to claim 1, wherein the method comprises the steps of: the combustion temperature in the high-temperature furnace is controlled to be 950+/-5 ℃.
4. The method for measuring the nitrogen content in the carbon-containing dust according to claim 1, wherein the method comprises the steps of: the temperature of the reduction furnace is controlled at 700+/-5 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310323878.8A CN116539659A (en) | 2023-03-29 | 2023-03-29 | Method for measuring nitrogen content in carbon-containing dust |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310323878.8A CN116539659A (en) | 2023-03-29 | 2023-03-29 | Method for measuring nitrogen content in carbon-containing dust |
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| CN116539659A true CN116539659A (en) | 2023-08-04 |
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| CN202310323878.8A Pending CN116539659A (en) | 2023-03-29 | 2023-03-29 | Method for measuring nitrogen content in carbon-containing dust |
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- 2023-03-29 CN CN202310323878.8A patent/CN116539659A/en active Pending
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