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 PDF

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Publication number
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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solution
hydrogen cyanide
sampling
coke
drexel bottle
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CN110470789B (en
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苏召飞
蒋淑敏
张光辉
徐苇
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Sichuan Daxing Energy Co ltd
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SICHUAN DAXING ENERGY CO Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/405Concentrating samples by adsorption or absorption
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating 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 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

The measuring method of hydrogen cyanide in a kind of coke-stove gas
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (19)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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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