CN110470789A - The measuring method of hydrogen cyanide in a kind of coke-stove gas - Google Patents
The measuring method of hydrogen cyanide in a kind of coke-stove gas Download PDFInfo
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- CN110470789A CN110470789A CN201910788697.6A CN201910788697A CN110470789A CN 110470789 A CN110470789 A CN 110470789A CN 201910788697 A CN201910788697 A CN 201910788697A CN 110470789 A CN110470789 A CN 110470789A
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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
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Abstract
The invention discloses a kind of measuring methods of hydrogen cyanide in coke-stove gas, belong to coke-stove gas analysis determining technology field.The present invention can simply, efficiently measure the hydrogen cyanide content after fine de-sulfur tower in coal gas by silver nitrate titration；Hydrogen sulfide content is high in coal gas before desulfurizing tower, using reducing coal gas uptake and increasing preposition lead acetate absorbing liquid, can also measure the hydrogen cyanide content before desulfurizing tower in coal gas.It can satisfy the routine analysis needs of factory using the hydrogen cyanide content that silver nitrate titration method is surveyed in coal gas, effectively Instructing manufacture.Since the solubility product constant of lead acetate is small, so selecting the interference of lead acetate removal hydrogen sulfide, effect is more satisfactory.
Description
Technical field
The present invention relates to coke-stove gas technical field of analysis and detection, and in particular to the measurement of hydrogen cyanide in a kind of coke-stove gas
Method.
Background technique
Although hydrogen cyanide content in coke-stove gas is few, there is a severe toxicity, when burning generates NOX, in gas purification process
In must remove, in coal gas cyanide content measurement as an important indicator during gas purification, it is necessary to surveyed
Amount and monitoring.Measurement hydrogen cyanide content does not have national standard and professional standard, and most common method is ammonium polysulfide method, the method
It is the most classic method that hydrogen cyanide measures in coal gas, accuracy is high, but the method step is complicated, and time-consuming, cannot refer in time
Production is led, reagent used is more, and plurality of reagents is poisonous and harmful, influences the physical and mental health of testing crew.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of measuring method of hydrogen cyanide in coke-stove gas,
Its is easy to operate, agents useful for same is few, detection accuracy is high.
The technical scheme to solve the above technical problems is that
The measuring method of hydrogen cyanide in a kind of coke-stove gas, comprising:
(1) after correcting wet gas flow meter, by gas piping, the pretreatment drexel bottle equipped with acetic acid lead solution, dress
The sampling drexel bottle and wet gas flow meter for having sodium hydroxide solution are sequentially communicated by appendix, are opened and are arranged in coal gas
Coal gas, is successively passed through the pretreatment drexel bottle by the valve on pipeline and sampling drexel bottle is sampled, and controls gas flow
For 1-2L/min, sample volume 50-60L, after sampling, the reading and coal gas of the wet gas flow meter are recorded
Temperature and pressure；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 1-2min is boiled in heating, cooling to solution
Liquid is transferred in volumetric flask afterwards；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned into beaker, then
Cleaning solution is again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up, obtains sample
Liquid；
(3) take the sample liquid in clean conical flask, be added dropwise when shaking acetic acid lead solution until solution in black precipitate not
It is generated until generating white precipitate again, filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then dripped with silver nitrate standard solution
It is fixed, it is titrated until solution becomes orange red stopping by yellow, records the consumption of silver nitrate solution, calculated according to the following formula burnt
The content of hydrogen cyanide in producer gas:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
F is also referred to as meter factor.
Further, in step (1), the concentration for pre-processing the acetic acid lead solution in drexel bottle is 40-60g/L, and volume is
80-120mL, the concentration for sampling the sodium hydroxide solution in drexel bottle is 15-25wt%, volume 80-120mL.
Further, in step (1), the concentration for pre-processing the acetic acid lead solution in drexel bottle is 50g/L, and volume is
100mL, the concentration for sampling the sodium hydroxide solution in drexel bottle is 20wt%, volume 100mL.
Further, in step (2), the specification of volumetric flask is 500mL.
Further, the concentration of the acetic acid lead solution in step (3) is 40-60g/L.
Further, the concentration of the acetic acid lead solution in step (3) is 50g/L.
Further, in step (4), the concentration of silver nitrate standard solution is 0.01-0.03mol/L.
Further, in step (4), the concentration of silver nitrate standard solution is 0.02mol/L.
The invention has the following advantages:
The present invention before sampling by setting the pretreatment drexel bottle containing acetic acid lead solution to the hydrogen sulfide in coal gas into
Row absorbs, and is substantially reduced hydrogen sulfide content in the coal gas entered in sampling drexel bottle, avoids hydrogen sulfide content to analysis result
Influence, and the present invention carries out heating to sample liquid after sampling and boils, and can remove ammoniacal substance in sample liquid and remnants
Hydrogen sulfide further increases detection accuracy.The present invention is removed in coal gas by different modes respectively before sampling and after sampling
The hydrogen sulfide and ammonia of testing result are influenced, the factor considered is mainly based upon before desulfurizing tower that hydrogen sulfide content is high in coal gas, such as
By the way of fruit is still eliminated with lead acetate after sampling again, lead acetate dosage used is more, causes pH value < 11 of titrating solution,
It is unsatisfactory for determination condition, to can not titrate, therefore, the present invention is removed before sampling, while being removed before sampling, moreover it is possible to
The sampling amount of coal gas is enough reduced, can be measured with the sample volume of original half.
The present invention can simply, efficiently measure the hydrogen cyanide content after fine de-sulfur tower in coal gas by silver nitrate titration；
Hydrogen sulfide content is high in coal gas before desulfurizing tower, using reducing coal gas uptake and increasing preposition lead acetate absorbing liquid, can also survey
Hydrogen cyanide content before desulfurizing tower in coal gas out.Factory can satisfy using the hydrogen cyanide content that silver nitrate titration method is surveyed in coal gas
Routine analysis need, effectively Instructing manufacture.Since the solubility product constant of lead acetate is small, so it is vulcanisation to select lead acetate to go
The interference of hydrogen, effect are more satisfactory.
Present invention reduces analytical cycles, improve accuracy of analysis, eliminate hydrogen sulfide content in coal gas and tie to analysis
The influence of fruit, measurement result favorable reproducibility, accuracy and precision as a result are able to satisfy the needs of production control.
Specific embodiment
Principles and features of the present invention are described with reference to embodiments, the given examples are served only to explain the present invention,
It is not intended to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer suggests
Condition carries out.Reagents or instruments used without specified manufacturer is the conventional products that can be obtained by commercially available purchase.
Embodiment 1:
The measuring method of hydrogen cyanide in the coke-stove gas of the present embodiment, comprising:
(1) wet gas flow meter is corrected, simultaneously air-dispersing 5min is connected to gas piping, by gas piping, acetic acid is housed
Pretreatment drexel bottle, the sampling drexel bottle equipped with sodium hydroxide solution and the wet gas flow meter of lead solution pass through appendix
It is sequentially communicated；The concentration of acetic acid lead solution is 40g/L, and volume 120mL, the concentration of sodium hydroxide solution is 15wt%, volume
For 120mL；
The valve being arranged on gas piping is opened, coal gas is successively passed through to the pretreatment drexel bottle and sampling drexel bottle
It is sampled, control gas flow is 1L/min, sample volume 50L, after sampling, records the wet gas flow meter
Reading and coal gas temperature and pressure；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 1min is boiled in heating, after solution is cooling
Liquid is transferred in 500ml volumetric flask；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned into beaker,
Then cleaning solution is again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up, obtain
Sample liquid；
(3) it takes the sample liquid in clean conical flask, the acetic acid lead solution that concentration is 40g/L is added dropwise when shaking until solution
Middle black precipitate no longer generates until generating white precipitate, and filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then 0.01mol/L's with concentration
Silver nitrate standard solution titration titrates until solution becomes orange red stopping by yellow, records the consumption of silver nitrate solution, press
The content of hydrogen cyanide in coke-stove gas is calculated according to following equation:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
Embodiment 2:
The measuring method of hydrogen cyanide in the coke-stove gas of the present embodiment, comprising:
(1) wet gas flow meter is corrected, simultaneously air-dispersing 10min is connected to gas piping, by gas piping, acetic acid is housed
Pretreatment drexel bottle, the sampling drexel bottle equipped with sodium hydroxide solution and the wet gas flow meter of lead solution pass through appendix
It is sequentially communicated；The concentration of acetic acid lead solution is 60g/L, and the concentration of volume 80mL, sodium hydroxide solution are 25wt%, and volume is
80mL；
The valve being arranged on gas piping is opened, coal gas is successively passed through to the pretreatment drexel bottle and sampling drexel bottle
It is sampled, control gas flow is 2L/min, sample volume 60L, after sampling, records the wet gas flow meter
Reading and coal gas temperature and pressure；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 2min is boiled in heating, after solution is cooling
Liquid is transferred in 500ml volumetric flask；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned into beaker,
Then cleaning solution is again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up, obtain
Sample liquid；
(3) it takes the sample liquid in clean conical flask, the acetic acid lead solution that concentration is 60g/L is added dropwise when shaking until solution
Middle black precipitate no longer generates until generating white precipitate, and filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then 0.03mol/L's with concentration
Silver nitrate standard solution titration titrates until solution becomes orange red stopping by yellow, records the consumption of silver nitrate solution, press
The content of hydrogen cyanide in coke-stove gas is calculated according to following equation:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
Embodiment 3:
The measuring method of hydrogen cyanide in the coke-stove gas of the present embodiment, comprising:
(1) wet gas flow meter is corrected, simultaneously air-dispersing 8min is connected to gas piping, by gas piping, acetic acid is housed
Pretreatment drexel bottle, the sampling drexel bottle equipped with sodium hydroxide solution and the wet gas flow meter of lead solution pass through appendix
It is sequentially communicated；The concentration of acetic acid lead solution is 50g/L, and volume 100mL, the concentration of sodium hydroxide solution is 20wt%, volume
For 100mL；
The valve being arranged on gas piping is opened, coal gas is successively passed through to the pretreatment drexel bottle and sampling drexel bottle
It is sampled, control gas flow is 1.5L/min, sample volume 55L, after sampling, records the wet gas flow
The reading of meter and the temperature and pressure of coal gas；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 1.5min is boiled in heating, cooling to solution
Liquid is transferred in 500ml volumetric flask afterwards；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned and is burnt
Cleaning solution, is then again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up by cup,
Obtain sample liquid；
(3) it takes the sample liquid in clean conical flask, the acetic acid lead solution that concentration is 50g/L is added dropwise when shaking until solution
Middle black precipitate no longer generates until generating white precipitate, and filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then 0.02mol/L's with concentration
Silver nitrate standard solution titration titrates until solution becomes orange red stopping by yellow, records the consumption of silver nitrate solution, press
The content of hydrogen cyanide in coke-stove gas is calculated according to following equation:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
Embodiment 4:
The measuring method of hydrogen cyanide in the coke-stove gas of the present embodiment, comprising:
(1) wet gas flow meter is corrected, simultaneously air-dispersing 10min is connected to gas piping, by gas piping, acetic acid is housed
Pretreatment drexel bottle, the sampling drexel bottle equipped with sodium hydroxide solution and the wet gas flow meter of lead solution pass through appendix
It is sequentially communicated；The concentration of acetic acid lead solution is 50g/L, and volume 100mL, the concentration of sodium hydroxide solution is 20wt%, volume
For 100mL；
The valve being arranged on gas piping is opened, coal gas is successively passed through to the pretreatment drexel bottle and sampling drexel bottle
It is sampled, control gas flow is 2L/min, sample volume 60L, after sampling, records the wet gas flow meter
Reading and coal gas temperature and pressure；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 2min is boiled in heating, after solution is cooling
Liquid is transferred in 500ml volumetric flask；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned into beaker,
Then cleaning solution is again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up, obtain
Sample liquid；
(3) it takes the sample liquid in clean conical flask, the acetic acid lead solution that concentration is 50g/L is added dropwise when shaking until solution
Middle black precipitate no longer generates until generating white precipitate, and filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then 0.02mol/L's with concentration
Silver nitrate standard solution titration titrates until solution becomes orange red stopping by yellow, records the consumption of silver nitrate solution, press
The content of hydrogen cyanide in coke-stove gas is calculated according to following equation:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
Embodiment 5:
The measuring method of hydrogen cyanide in the coke-stove gas of the present embodiment, comprising:
(1) wet gas flow meter is corrected, simultaneously air-dispersing 10min is connected to gas piping, by gas piping, acetic acid is housed
Pretreatment drexel bottle, the sampling drexel bottle equipped with sodium hydroxide solution and the wet gas flow meter of lead solution pass through appendix
It is sequentially communicated；The concentration of acetic acid lead solution is 50g/L, and volume 100mL, the concentration of sodium hydroxide solution is 20wt%, volume
For 100mL；
The valve being arranged on gas piping is opened, coal gas is successively passed through to the pretreatment drexel bottle and sampling drexel bottle
It is sampled, control gas flow is 2L/min, sample volume 50L, after sampling, records the wet gas flow meter
Reading and coal gas temperature and pressure；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 2min is boiled in heating, after solution is cooling
Liquid is transferred in 500ml volumetric flask；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned into beaker,
Then cleaning solution is again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up, obtain
Sample liquid；
(3) it takes the sample liquid in clean conical flask, the acetic acid lead solution that concentration is 50g/L is added dropwise when shaking until solution
Middle black precipitate no longer generates until generating white precipitate, and filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then 0.02mol/L's with concentration
Silver nitrate standard solution titration titrates until solution becomes orange red stopping by yellow, records the consumption of silver nitrate solution, press
The content of hydrogen cyanide in coke-stove gas is calculated according to following equation:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
Embodiment 6:
The measuring method of hydrogen cyanide in the coke-stove gas of the present embodiment, comprising:
(1) wet gas flow meter is corrected, simultaneously air-dispersing 5min is connected to gas piping, by gas piping, acetic acid is housed
Pretreatment drexel bottle, the sampling drexel bottle equipped with sodium hydroxide solution and the wet gas flow meter of lead solution pass through appendix
It is sequentially communicated；The concentration of acetic acid lead solution is 50g/L, and volume 100mL, the concentration of sodium hydroxide solution is 20wt%, volume
For 100mL；
The valve being arranged on gas piping is opened, coal gas is successively passed through to the pretreatment drexel bottle and sampling drexel bottle
It is sampled, control gas flow is 1L/min, sample volume 50L, after sampling, records the wet gas flow meter
Reading and coal gas temperature and pressure；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 2min is boiled in heating, after solution is cooling
Liquid is transferred in 500ml volumetric flask；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned into beaker,
Then cleaning solution is again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up, obtain
Sample liquid；
(3) it takes the sample liquid in clean conical flask, the acetic acid lead solution that concentration is 50g/L is added dropwise when shaking until solution
Middle black precipitate no longer generates until generating white precipitate, and filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then 0.02mol/L's with concentration
Silver nitrate standard solution titration titrates until solution becomes orange red stopping by yellow, records the consumption of silver nitrate solution, press
The content of hydrogen cyanide in coke-stove gas is calculated according to following equation:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
The result of above-described embodiment measurement is counted in table 1.
Hydrogen cyanide content in coal gas before 1 desulfurizing tower of table
The embodiment of the present invention can carry out hydrogen cyanide detection to the coal gas before desulfurizing tower, reduce and absorb gas volume, can be effective
Measure hydrogen cyanide content in coal gas.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. the measuring method of hydrogen cyanide in a kind of coke-stove gas characterized by comprising
(1) after correcting wet gas flow meter, by gas piping, the pretreatment drexel bottle equipped with acetic acid lead solution, hydrogen is housed
The sampling drexel bottle of sodium hydroxide solution and wet gas flow meter are sequentially communicated by appendix, are opened and are arranged in gas piping
On valve, coal gas is successively passed through the pretreatment drexel bottle and sampling drexel bottle be sampled, control gas flow be 1-
2L/min, sample volume 50-60L after sampling, record the reading of the wet gas flow meter and the temperature of coal gas
And pressure；
(2) absorbing liquid in the sampling drexel bottle is all moved into beaker, 1-2min is boiled in heating, will after solution is cooling
Liquid is transferred in volumetric flask；It is multiple to be washed with distilled water the sampling drexel bottle, wash liquid is cleaned into beaker, then will be washed
It washs liquid to be again transferred in the volumetric flask, then by the middle diluted absorption solution of volumetric flask to scale, shakes up, obtain sample liquid；
(3) it takes the sample liquid in clean conical flask, acetic acid lead solution is added dropwise when shaking until black precipitate no longer produces in solution
It is raw and until generating white precipitate, filtering obtains filtrate；
(4) it takes the filtrate in clean conical flask, p-dimethylaminobenzal rhodanine indicator is added, is then titrated with silver nitrate standard solution, directly
Become orange red stopping by yellow to solution to titrate, records the consumption of silver nitrate solution, calculate coke-oven coal according to the following formula
The content of hydrogen cyanide in gas:
In formula:
V-gas sampling volume, L；
Absorbing liquid sodium hydroxide solution dosage, mL in V1-sampling drexel bottle；
V3—AgNO3Standard solution dosage, mL；
F-air pressure correction correction factor；
M—AgNO3Concentration of standard solution, mol/L；
The molal weight of 0.054-hydrogen cyanide.
2. the measuring method of hydrogen cyanide in coke-stove gas according to claim 1, which is characterized in that pre- to locate in step (1)
The concentration for managing the acetic acid lead solution in drexel bottle is 40-60g/L, volume 80-120mL, samples the sodium hydroxide in drexel bottle
The concentration of solution is 15-25wt%, volume 80-120mL.
3. the measuring method of hydrogen cyanide in coke-stove gas according to claim 2, which is characterized in that pre- to locate in step (1)
The concentration for managing the acetic acid lead solution in drexel bottle is 50g/L, volume 100mL, samples the sodium hydroxide solution in drexel bottle
Concentration is 20wt%, volume 100mL.
4. the measuring method of hydrogen cyanide in coke-stove gas according to claim 1, which is characterized in that in step (2), capacity
The specification of bottle is 500mL.
5. the measuring method of hydrogen cyanide in coke-stove gas according to claim 1, which is characterized in that the vinegar in step (3)
The concentration of lead plumbate solution is 40-60g/L.
6. the measuring method of hydrogen cyanide in coke-stove gas according to claim 5, which is characterized in that the vinegar in step (3)
The concentration of lead plumbate solution is 50g/L.
7. the measuring method of hydrogen cyanide in coke-stove gas according to claim 1-6, which is characterized in that step
(4) in, the concentration of silver nitrate standard solution is 0.01-0.03mol/L.
8. the measuring method of hydrogen cyanide in coke-stove gas according to claim 7, which is characterized in that in step (4), nitric acid
The concentration of silver-colored standard solution is 0.02mol/L.
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Citations (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1038344A (en) * | 1962-12-14 | 1966-08-10 | Ciba Ltd | New benzo aza-cycloalkenes |
| EP0629684A1 (en) * | 1993-06-17 | 1994-12-21 | Texaco Development Corporation | Partial oxidation process for producing a stream of hot purified gas |
| US5958588A (en) * | 1997-02-05 | 1999-09-28 | Degussa-Huls Ag | Process for preparing alkali metal cyanide and alkaline earth metal cyanide granules and the high purity alkali metal cyanide granules obtainable thereby |
| WO2009126769A2 (en) * | 2008-04-09 | 2009-10-15 | Velocys Inc. | Process for upgrading a carbonaceous material using microchannel process technology |
| US20090294328A1 (en) * | 2008-05-28 | 2009-12-03 | Kellogg Brown & Root Llc | Integrated solven deasphalting and gasification |
| 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 |
| US20120195795A1 (en) * | 2009-08-03 | 2012-08-02 | Voestalpine Stahl Gmbh | Method for continuously determining the concentration of at least one cn compound in an aqueous solution |
| 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 |
| CN105784696A (en) * | 2016-03-07 | 2016-07-20 | 贵州大学 | Method for analyzing and measuring sulfur of all valence states in 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 |
| 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 |
-
2019
- 2019-08-26 CN CN201910788697.6A patent/CN110470789B/en active Active
Patent Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1038344A (en) * | 1962-12-14 | 1966-08-10 | Ciba Ltd | New benzo aza-cycloalkenes |
| 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 |
| US5958588A (en) * | 1997-02-05 | 1999-09-28 | Degussa-Huls Ag | Process for preparing alkali metal cyanide and alkaline earth metal cyanide granules and the high purity alkali metal cyanide granules obtainable thereby |
| WO2009126769A2 (en) * | 2008-04-09 | 2009-10-15 | Velocys Inc. | Process for upgrading a carbonaceous material using microchannel process technology |
| US20090294328A1 (en) * | 2008-05-28 | 2009-12-03 | Kellogg Brown & Root Llc | Integrated solven deasphalting and gasification |
| US20120195795A1 (en) * | 2009-08-03 | 2012-08-02 | Voestalpine Stahl Gmbh | Method for continuously determining the concentration of at least one cn compound in an aqueous solution |
| 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 |
| CN105784696A (en) * | 2016-03-07 | 2016-07-20 | 贵州大学 | Method for analyzing and measuring sulfur of all valence states in 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 |
| 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 (9)
| Title |
|---|
| SHOKUHI RAD ALI ETC: "The polythiophene molecular segment as a sensor model for H2O, HCN, NH3, SO3, and H2S: a density functional theory study", 《 JOURNAL OF MOLECULAR MODELING》 * |
| 任东等: "微浓度过氧化氢的快速分光光度法检测", 《现代化工》 * |
| 宫崎正葳: "《无机化学例题与习题》", 31 May 1980, 人民教育出版社 * |
| 杨建华: "《焦炉煤气净化》", 31 December 2005, 北京：化学工业出版 * |
| 王光荣: "《分析化学学习指导及习题解答》", 30 November 2018, 中国科学技术大学出版社 * |
| 王国强: "《制药工艺学》", 31 August 2017, 中国中医药出版社 * |
| 韩昌贵: "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", 《化工管理》 * |
| 龙旭等: "水蒸气重整制氢技术研究进展", 《科技展望》 * |
| 龙素安等: "焦炉煤气HPF氨法脱硫装置优化改造", 《燃料与化工》 * |
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