CN110470789B - Method for determining hydrogen cyanide in coke oven gas - Google Patents
Method for determining hydrogen cyanide in coke oven gas Download PDFInfo
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- CN110470789B CN110470789B CN201910788697.6A CN201910788697A CN110470789B CN 110470789 B CN110470789 B CN 110470789B CN 201910788697 A CN201910788697 A CN 201910788697A CN 110470789 B CN110470789 B CN 110470789B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
Abstract
The invention discloses a method for measuring hydrogen cyanide in coke oven gas, and belongs to the technical field of analysis and measurement of coke oven gas. According to the method, the content of the hydrogen cyanide in the coal gas after the fine desulfurization tower can be simply and quickly measured through silver nitrate titration; the content of hydrogen sulfide in the coal gas in front of the desulfurizing tower is high, and the content of hydrogen cyanide in the coal gas in front of the desulfurizing tower can be measured by reducing the absorption amount of the coal gas and increasing the lead acetate absorption liquid. The hydrogen cyanide content in the gas is measured by a silver nitrate titration method, so that the daily analysis requirement of a factory can be met, and the production is effectively guided. Because the solubility product constant of the lead acetate is small, the lead acetate is selected to remove the interference of the hydrogen sulfide, and the effect is relatively ideal.
Description
Technical Field
The invention relates to the technical field of analysis and detection of coke oven gas, in particular to a method for determining hydrogen cyanide in coke oven gas.
Background
Although the content of hydrogen cyanide in the coke oven gas is not much, the hydrogen cyanide is extremely toxic, NOx is generated during combustion, the hydrogen cyanide must be removed in the gas purification process, and the measurement of the cyanide content in the gas is taken as an important index in the gas purification process and must be measured and monitored. The method for measuring the content of the hydrogen cyanide has no national standard and industrial standard, the most common method is an ammonium polysulfide method, the method is the most classical method for measuring the hydrogen cyanide in the coal gas, the accuracy is high, but the method has complex steps, takes long time, cannot guide the production in time, uses a large amount of reagents, and various reagents are toxic and harmful, so that the physical and mental health of testers is influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for measuring hydrogen cyanide in coke oven gas, which is simple to operate, uses less reagents and has high detection precision.
The technical scheme for solving the technical problems is as follows:
a method for measuring hydrogen cyanide in coke oven gas comprises the following steps:
(1) after the wet gas flowmeter is corrected, sequentially communicating a gas pipeline, a pretreatment gas washing bottle filled with a lead acetate solution, a sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas transmission pipe, opening a valve arranged on the gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 1-2L/min and the sampling volume to be 50-60L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 1-2min, and transferring the liquid into a volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a lead acetate solution while shaking until no black precipitate is generated in the solution and a white precipitate is generated, and filtering to obtain a filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3standard solution dosage, mL;
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide.
f is also referred to as a flow meter calibration factor.
Further, in the step (1), the concentration of the lead acetate solution in the pretreatment gas washing bottle is 40-60g/L, the volume is 80-120mL, and the concentration of the sodium hydroxide solution in the sampling gas washing bottle is 15-25 wt%, and the volume is 80-120 mL.
Further, in the step (1), the concentration of the lead acetate solution in the pretreatment gas washing bottle is 50g/L, the volume is 100mL, and the concentration of the sodium hydroxide solution in the sampling gas washing bottle is 20 wt%, and the volume is 100 mL.
Further, in the step (2), the volume bottle has a standard of 500 mL.
Further, the concentration of the lead acetate solution in the step (3) is 40-60 g/L.
Further, the concentration of the lead acetate solution in the step (3) is 50 g/L.
Further, in the step (4), the concentration of the silver nitrate standard solution is 0.01-0.03 mol/L.
Further, in the step (4), the concentration of the silver nitrate standard solution is 0.02 mol/L.
The invention has the following beneficial effects:
according to the invention, the pretreatment gas washing bottle containing the lead acetate solution is arranged to absorb the hydrogen sulfide in the gas before sampling, so that the content of the hydrogen sulfide in the gas entering the sampling gas washing bottle is obviously reduced, and the influence of the content of the hydrogen sulfide on an analysis result is avoided. The invention removes hydrogen sulfide and ammonia which affect the detection result in the coal gas respectively before and after sampling, the considered factors are mainly based on the high content of hydrogen sulfide in the coal gas before the desulfurizing tower, if the method of removing lead acetate after sampling is still adopted, the used lead acetate is more, the PH value of the titration liquid is less than 11, the determination condition is not satisfied, and the titration cannot be performed, therefore, the invention removes the hydrogen sulfide and the ammonia before sampling, and simultaneously removes the hydrogen sulfide and the ammonia before sampling, and can reduce the sampling amount of the coal gas, and can determine by half of the original sampling volume.
According to the method, the content of the hydrogen cyanide in the coal gas after the fine desulfurization tower can be simply and quickly measured through silver nitrate titration; the content of hydrogen sulfide in the coal gas in front of the desulfurizing tower is high, and the content of hydrogen cyanide in the coal gas in front of the desulfurizing tower can be measured by reducing the absorption amount of the coal gas and increasing the lead acetate absorption liquid. The hydrogen cyanide content in the gas is measured by a silver nitrate titration method, so that the daily analysis requirement of a factory can be met, and the production is effectively guided. Because the solubility product constant of the lead acetate is small, the lead acetate is selected to remove the interference of the hydrogen sulfide, and the effect is relatively ideal.
The invention shortens the analysis period, improves the analysis accuracy, eliminates the influence of the content of the hydrogen sulfide in the coal gas on the analysis result, has good reproducibility of the determination result, and can meet the requirement of production control on the accuracy and precision of the result.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
the method for measuring hydrogen cyanide in coke oven gas of the embodiment comprises the following steps:
(1) correcting the wet gas flowmeter, communicating the wet gas flowmeter with a gas pipeline and exhausting gas for 5min, and sequentially communicating the gas pipeline, the pretreatment gas washing bottle filled with a lead acetate solution, the sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas conveying pipe; the concentration of the lead acetate solution is 40g/L, the volume is 120mL, the concentration of the sodium hydroxide solution is 15 wt%, and the volume is 120 mL;
opening a valve arranged on a gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 1L/min and the sampling volume to be 50L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling is finished;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 1min, and transferring the liquid into a 500ml volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a 40g/L lead acetate solution while shaking until no black precipitate is generated in the solution and a white precipitate is generated, and filtering to obtain a filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution with the concentration of 0.01mol/L until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3standard solution dosage, mL;
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide.
Example 2:
the method for measuring hydrogen cyanide in coke oven gas of the embodiment comprises the following steps:
(1) correcting the wet gas flowmeter, communicating the wet gas flowmeter with a gas pipeline and exhausting gas for 10min, and sequentially communicating the gas pipeline, the pretreatment gas washing bottle filled with a lead acetate solution, the sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas conveying pipe; the concentration of the lead acetate solution is 60g/L, the volume is 80mL, the concentration of the sodium hydroxide solution is 25 wt%, and the volume is 80 mL;
opening a valve arranged on a gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 2L/min and the sampling volume to be 60L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling is finished;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 2min, and transferring the liquid into a 500ml volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a 60g/L lead acetate solution while shaking until no black precipitate is generated in the solution and a white precipitate is generated, and filtering to obtain a filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution with the concentration of 0.03mol/L until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3amount of Standard solution, mL；
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide.
Example 3:
the method for measuring hydrogen cyanide in coke oven gas of the embodiment comprises the following steps:
(1) correcting the wet gas flowmeter, communicating the wet gas flowmeter with a gas pipeline and exhausting gas for 8min, and sequentially communicating the gas pipeline, the pretreatment gas washing bottle filled with a lead acetate solution, the sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas conveying pipe; the concentration of the lead acetate solution is 50g/L, the volume is 100mL, the concentration of the sodium hydroxide solution is 20 wt%, and the volume is 100 mL;
opening a valve arranged on a gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 1.5L/min and the sampling volume to be 55L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling is finished;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 1.5min, and transferring the liquid into a 500ml volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a lead acetate solution with the concentration of 50g/L while shaking until no black precipitate is generated in the solution and a white precipitate is generated, and filtering to obtain a filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution with the concentration of 0.02mol/L until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3standard solution dosage, mL;
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide.
Example 4:
the method for measuring hydrogen cyanide in coke oven gas of the embodiment comprises the following steps:
(1) correcting the wet gas flowmeter, communicating the wet gas flowmeter with a gas pipeline and exhausting gas for 10min, and sequentially communicating the gas pipeline, the pretreatment gas washing bottle filled with a lead acetate solution, the sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas conveying pipe; the concentration of the lead acetate solution is 50g/L, the volume is 100mL, the concentration of the sodium hydroxide solution is 20 wt%, and the volume is 100 mL;
opening a valve arranged on a gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 2L/min and the sampling volume to be 60L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling is finished;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 2min, and transferring the liquid into a 500ml volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a lead acetate solution with the concentration of 50g/L while shaking until no black precipitate is generated in the solution and a white precipitate is generated, and filtering to obtain a filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution with the concentration of 0.02mol/L until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3standard solution dosage, mL;
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide.
Example 5:
the method for measuring hydrogen cyanide in coke oven gas of the embodiment comprises the following steps:
(1) correcting the wet gas flowmeter, communicating the wet gas flowmeter with a gas pipeline and exhausting gas for 10min, and sequentially communicating the gas pipeline, the pretreatment gas washing bottle filled with a lead acetate solution, the sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas conveying pipe; the concentration of the lead acetate solution is 50g/L, the volume is 100mL, the concentration of the sodium hydroxide solution is 20 wt%, and the volume is 100 mL;
opening a valve arranged on a gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 2L/min and the sampling volume to be 50L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling is finished;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 2min, and transferring the liquid into a 500ml volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a lead acetate solution with the concentration of 50g/L while shaking until black precipitates in the solution are not generated any more and white precipitates are generated, and filtering to obtain filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution with the concentration of 0.02mol/L until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3standard solution dosage, mL;
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide.
Example 6:
the method for measuring hydrogen cyanide in coke oven gas of the embodiment comprises the following steps:
(1) correcting the wet gas flowmeter, communicating the wet gas flowmeter with a gas pipeline and exhausting gas for 5min, and sequentially communicating the gas pipeline, the pretreatment gas washing bottle filled with a lead acetate solution, the sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas conveying pipe; the concentration of the lead acetate solution is 50g/L, the volume is 100mL, the concentration of the sodium hydroxide solution is 20 wt%, and the volume is 100 mL;
opening a valve arranged on a gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 1L/min and the sampling volume to be 50L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling is finished;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 2min, and transferring the liquid into a 500ml volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a lead acetate solution with the concentration of 50g/L while shaking until no black precipitate is generated in the solution and a white precipitate is generated, and filtering to obtain a filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution with the concentration of 0.02mol/L until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3standard solution dosage, mL;
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide.
The results of the measurements in the above examples are summarized in Table 1.
TABLE 1 hydrogen cyanide content in the front gas of the desulfurization tower
The embodiment of the invention can detect the hydrogen cyanide in the coal gas in front of the desulfurizing tower, reduce the amount of the absorbed coal gas and effectively measure the content of the hydrogen cyanide in the coal gas.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A method for measuring hydrogen cyanide in coke oven gas is characterized by comprising the following steps:
(1) after the wet gas flowmeter is corrected, sequentially communicating a gas pipeline, a pretreatment gas washing bottle filled with a lead acetate solution, a sampling gas washing bottle filled with a sodium hydroxide solution and the wet gas flowmeter through a gas transmission pipe, opening a valve arranged on the gas pipeline, sequentially introducing gas into the pretreatment gas washing bottle and the sampling gas washing bottle for sampling, controlling the gas flow to be 1-2L/min and the sampling volume to be 50-60L, and recording the reading of the wet gas flowmeter and the temperature and pressure of the gas after sampling is finished;
(2) transferring all the absorption liquid in the sampling gas washing bottle into a beaker, heating and boiling for 1-2min, and transferring the liquid into a volumetric flask after the solution is cooled; washing the sampling gas washing bottle with distilled water for multiple times, washing a beaker with washing liquid, transferring the washing liquid into the volumetric flask again, diluting the middle absorption liquid in the volumetric flask to a scale, and shaking up to obtain a sample liquid;
(3) putting the sample solution into a clean conical flask, dropwise adding a lead acetate solution while shaking until no black precipitate is generated in the solution and a white precipitate is generated, and filtering to obtain a filtrate;
(4) putting the filtrate into a clean conical flask, adding a silver test indicator, titrating with a silver nitrate standard solution until the solution changes from yellow to orange red, stopping titrating, recording the consumption of the silver nitrate solution, and calculating the content of hydrogen cyanide in the coke oven gas according to the following formula:
in the formula:
v is the gas sampling volume, L;
v1-the amount of absorption liquid sodium hydroxide solution in the sampling gas washing bottle, mL;
V3—AgNO3standard solution dosage, mL;
f, correcting factor for air pressure correction;
M—AgNO3concentration of standard solution, mol/L;
0.054-molar mass of hydrogen cyanide;
in the step (1), the concentration of the lead acetate solution in the pretreated gas washing bottle is 40-60g/L, the volume of the lead acetate solution is 80-120mL, the concentration of the sodium hydroxide solution in the sampling gas washing bottle is 15-25 wt%, and the volume of the sodium hydroxide solution is 80-120 mL; the concentration of the lead acetate solution in the step (3) is 40-60 g/L.
2. The method for determining hydrogen cyanide in coke oven gas according to claim 1, wherein in the step (1), the concentration of the lead acetate solution in the pretreatment gas washing bottle is 50g/L, the volume is 100mL, and the concentration of the sodium hydroxide solution in the sampling gas washing bottle is 20 wt%, and the volume is 100 mL.
3. The method for measuring hydrogen cyanide in coke oven gas as claimed in claim 1, wherein in the step (2), the volume flask has a size of 500 mL.
4. The method for determining hydrogen cyanide in coke oven gas as claimed in claim 1, wherein the concentration of the lead acetate solution in the step (3) is 50 g/L.
5. The method for determining hydrogen cyanide in coke oven gas as claimed in any one of claims 1 to 4, wherein in the step (4), the concentration of the silver nitrate standard solution is 0.01 to 0.03 mol/L.
6. The method for determining hydrogen cyanide in coke oven gas according to claim 5, wherein in the step (4), the concentration of the silver nitrate standard solution is 0.02 mol/L.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0629684A1 (en) * | 1993-06-17 | 1994-12-21 | Texaco Development Corporation | Partial oxidation process for producing a stream of hot purified gas |
| CN101781010A (en) * | 2010-03-17 | 2010-07-21 | 湖南国发精细化工科技有限公司 | Novel treatment process for cyclic utilization of high-concentration sodium cyanide-containing waste water |
| CN102079689A (en) * | 2009-11-30 | 2011-06-01 | 四川达兴能源股份有限公司 | Method and equipment for producing methanol |
| CN102607900A (en) * | 2012-03-21 | 2012-07-25 | 云南昆钢煤焦化有限公司 | Coal gas sampling method for determining content of hydrogen cyanide in coal gas |
| CN102636616A (en) * | 2012-03-21 | 2012-08-15 | 云南昆钢煤焦化有限公司 | Method for testing content of hydrogen cyanide in gas |
| CN202494586U (en) * | 2012-03-21 | 2012-10-17 | 云南昆钢煤焦化有限公司 | Gas sampling device |
| CN102798124A (en) * | 2012-08-22 | 2012-11-28 | 四川达兴能源股份有限公司 | Gas combustion method for primary reformer of methanol device and combustor for reformer |
| CN103071370A (en) * | 2013-01-24 | 2013-05-01 | 昆明理工大学 | Method and device for purifying hydrogen cyanide industrial waste gas by electrodialysis |
| CN105000738A (en) * | 2015-07-13 | 2015-10-28 | 四川达兴能源股份有限公司 | Method for reducing content of salt in desulfurization waste liquor |
| CN108489978A (en) * | 2018-03-22 | 2018-09-04 | 长春黄金研究院有限公司 | The assay method of total sulfur in a kind of cyanating solution |
| CN108793509A (en) * | 2018-07-15 | 2018-11-13 | 长春黄金研究院有限公司 | A kind of method of cyanidation tailings cycle of higher pressure countercurrent washing recovery of cyanide |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL301813A (en) * | 1962-12-14 | 1900-01-01 | ||
| DE19704180C1 (en) * | 1997-02-05 | 1998-08-20 | Degussa | Process for the preparation of alkali cyanide and alkaline earth cyanide granules and alkali cyanide granules of high purity obtainable here |
| CN105749831A (en) * | 2008-04-09 | 2016-07-13 | 万罗赛斯公司 | Process For Upgrading Carbonaceous Material By Using Microchannel Process Technology |
| US7964090B2 (en) * | 2008-05-28 | 2011-06-21 | Kellogg Brown & Root Llc | Integrated solvent deasphalting and gasification |
| AT508502B1 (en) * | 2009-08-03 | 2011-03-15 | Voestalpine Stahl Gmbh | METHOD AND DEVICE FOR CONTINUOUS DETERMINATION OF THE LEVEL OF AT LEAST ONE CN COMPOUND IN AN AQUEOUS SOLUTION |
| CN105784696B (en) * | 2016-03-07 | 2018-08-21 | 贵州大学 | The analysis determining method of each valence state sulphur in a kind of sodium aluminate solution |
| CN107271596A (en) * | 2017-07-12 | 2017-10-20 | 云南中烟工业有限责任公司 | A kind of method of hydrogen sulfide content in hydrogen sulfide separator and detection medicinal extract spices |
-
2019
- 2019-08-26 CN CN201910788697.6A patent/CN110470789B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0629684A1 (en) * | 1993-06-17 | 1994-12-21 | Texaco Development Corporation | Partial oxidation process for producing a stream of hot purified gas |
| US5403366A (en) * | 1993-06-17 | 1995-04-04 | Texaco Inc. | Partial oxidation process for producing a stream of hot purified gas |
| CN102079689A (en) * | 2009-11-30 | 2011-06-01 | 四川达兴能源股份有限公司 | Method and equipment for producing methanol |
| CN101781010A (en) * | 2010-03-17 | 2010-07-21 | 湖南国发精细化工科技有限公司 | Novel treatment process for cyclic utilization of high-concentration sodium cyanide-containing waste water |
| CN102607900A (en) * | 2012-03-21 | 2012-07-25 | 云南昆钢煤焦化有限公司 | Coal gas sampling method for determining content of hydrogen cyanide in coal gas |
| CN102636616A (en) * | 2012-03-21 | 2012-08-15 | 云南昆钢煤焦化有限公司 | Method for testing content of hydrogen cyanide in gas |
| CN202494586U (en) * | 2012-03-21 | 2012-10-17 | 云南昆钢煤焦化有限公司 | Gas sampling device |
| CN102798124A (en) * | 2012-08-22 | 2012-11-28 | 四川达兴能源股份有限公司 | Gas combustion method for primary reformer of methanol device and combustor for reformer |
| CN103071370A (en) * | 2013-01-24 | 2013-05-01 | 昆明理工大学 | Method and device for purifying hydrogen cyanide industrial waste gas by electrodialysis |
| CN105000738A (en) * | 2015-07-13 | 2015-10-28 | 四川达兴能源股份有限公司 | Method for reducing content of salt in desulfurization waste liquor |
| CN108489978A (en) * | 2018-03-22 | 2018-09-04 | 长春黄金研究院有限公司 | The assay method of total sulfur in a kind of cyanating solution |
| CN108793509A (en) * | 2018-07-15 | 2018-11-13 | 长春黄金研究院有限公司 | A kind of method of cyanidation tailings cycle of higher pressure countercurrent washing recovery of cyanide |
Non-Patent Citations (1)
| Title |
|---|
| 水质氰化物的测定异烟酸-吡唑啉酮分光光度法 （HJ 484-2009）对工业污水检测方法验证;韩昌贵;《化工管理》;20140409(第6期);第94页 * |
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Address after: Dazhou City, Sichuan Province, 635000 River Road District No. 25 Patentee after: Sichuan Daxing Energy Co.,Ltd. Address before: Dazhou City, Sichuan Province, 635000 River Road District No. 25 Patentee before: SICHUAN DAXING ENERGY Co.,Ltd. |