CN102636616A - Method for testing content of hydrogen cyanide in gas - Google Patents

Method for testing content of hydrogen cyanide in gas Download PDF

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Publication number
CN102636616A
CN102636616A CN2012100746408A CN201210074640A CN102636616A CN 102636616 A CN102636616 A CN 102636616A CN 2012100746408 A CN2012100746408 A CN 2012100746408A CN 201210074640 A CN201210074640 A CN 201210074640A CN 102636616 A CN102636616 A CN 102636616A
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solution
volume
sample
silver nitrate
gas
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Inventor
尹思聪
张丕祥
龙菊兴
徐东升
毛艾萍
王自芳
张少平
王健
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YUNNAN KUNGANG COAL COKING CO Ltd
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YUNNAN KUNGANG COAL COKING CO Ltd
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Abstract

The invention provides a method for testing content of hydrogen cyanide in gas. The method comprises the following steps of: absorbing the hydrogen cyanide in the gas by adopting a potassium hydroxide solution, transferring the absorption solution to a volumetric flask with a certain volume, taking a certain amount of absorption solution, adding a cadmium acetate solution to make sulfide in the absorption solution to form indissolvable cadmium sulfide to sediment, filtering and sintering the absorption solution to eliminate the sediments, taking Dabr as an indicator of the solution, taking a standard silver nitrate solution to titrate, making cyanide ions react with silver nitrateto form soluble cyanide complex ion (Ag(CN)2), making excessive silver ions react with the Dabar indicator so as to make the color of the solution change from yellow to orange to the end, and calculating the content of the hydrogen cyanide according to the volume of the consumed standard silver nitrate solution. The method provided by the invention solves the problems that various kinds of reagents used in the prior art are poisonous and harmful, and moreover the reagents have the disadvantages of complex analysis step, long elapsed time and the like, have potential safety hazards existing in the testing process, and enhance the sewage treatment load of the back section. The method can rapidly and accurately test the content of the hydrogen cyanide in coke oven coal.

Description

The assay method of hydrogen cyanide content in the coal gas
?
Technical field
The present invention relates to a kind of assay method, the assay method of hydrogen cyanide content in particularly a kind of coke-oven gas belongs to coal tar fractional analysis technical field of measurement and test.
Background technology
Though sulfuretted hydrogen and hydrogen cyanide content in coke-oven gas is few, but objectionable constituent must remove.In the coke oven gas purification process; In order also to remove hydrogen cyanide in the sulfuretted hydrogen in removing coke-oven gas; Just need measure to the coal gas before the entering desulfurizer and through the coal gas that desulfurizer comes out; To confirm that the hydrogen cyanide in the coal gas removes situation, therefore, this determination data is an important indicator of gas purification.Yet in the prior art,, therefore bring inconvenience to enterprise because the assay method of hydrogen cyanide content does not have national standard and industry standard in the coal gas.In the prior art, the mensuration to hydrogen cyanide content in the forward and backward coal gas of desulfurizer adopts the ammonium polysulfide method usually; The method agents useful for same kind is more, and wherein has plurality of reagents to belong to the poisonous and harmful agent, healthy unfavorable to the analyst; Exist analytical procedure complicated simultaneously, problems such as length consuming time, and in the mensuration process; Chang Yinwei wants heating sample and has potential safety hazards such as electric shock, scald, poisoning and corrosion; In the waste liquid that this external mensuration process is produced,, thereby increased the load of postorder wastewater treatment because of poisonous and harmful element is many.Therefore, must improve prior art.
Summary of the invention
In order to solve the reagent poisonous and harmful that prior art exists, analytical procedure is complicated, length consuming time, and problem such as waste liquor contamination is heavier, the present invention provides the assay method of hydrogen cyanide content in a kind of coke-oven gas.
The present invention realizes through following technical proposal: the assay method of hydrogen cyanide content in a kind of coal gas is characterized in that through following each step:
(1) volume is
Figure 2012100746408100002DEST_PATH_IMAGE002
to feed coal gas to gas sampling in the potassium hydroxide solution that be 30～40% in mass concentration, volume is 100～120mL, must be absorbed with the sample absorption liquid of hydrogen cyanide;
(2) step (1) gained sample absorption liquid is diluted with water to 250mL; Shake up the sample dilution; Get this sample dilution 10mL; And drip no yellow sulfide-cadmium precipitation in the clear liquid of cadmium acetate solution to upper strata therein, and excessive till produce a small amount of white precipitate, make the sulfide in the sample absorption liquid form the sulfide-cadmium precipitation thing of indissoluble and get into lower floor; After the filtration; With distilled water cyclic washing sediment, to 100mL, in sample filtrating, add 3 of p-dimethylaminobenzal rhodanine indicator then until the sample filtrate volume of collecting; With silver nitrate standard solution titration sample filtrating to orange red, obtain silver nitrate standard solution that titration sample filtrating consumed volume is
Figure 2012100746408100002DEST_PATH_IMAGE004
;
(3) get 80mL water; And in water, to add the 4mL mass concentration be potassium hydroxide solution and 2 cadmium acetate solution of 30～40%; Add 3 p-dimethylaminobenzal rhodanine indicator again; The blank solution that shakes up yellowly; With the silver nitrate standard solution titration should yellow blank solution to orange red, obtain silver nitrate standard solution that the titration blank solution consumes volume is
Figure 2012100746408100002DEST_PATH_IMAGE006
;
(4) content through hydrogen cyanide in the computes coke-oven gas:
Figure 2012100746408100002DEST_PATH_IMAGE008
In the formula:
---the quality of suitable with 1.00mL silver nitrate standard solution (1.000 mol/L) hydrogen cyanide with the gram expression;
---the concentration of silver nitrate standard solution, mol/L;
Figure 726422DEST_PATH_IMAGE004
---the volume of the silver nitrate standard solution that titration sample filtrating is consumed, mL;
Figure 2012100746408100002DEST_PATH_IMAGE014
---the volume of the silver nitrate standard solution that the titration blank solution is consumed, mL;
Figure 269661DEST_PATH_IMAGE002
---be scaled 101.325KPa, the gas sampling volume 15 ℃ the time, L.
Gas sampling volume in the said step (1)
Figure 580556DEST_PATH_IMAGE002
is: the saturation vapor pressure W the when gas pressure
Figure 2012100746408100002DEST_PATH_IMAGE022
the when atmospheric pressure
Figure 2012100746408100002DEST_PATH_IMAGE020
during with conventional wet test meter metering sample volume
Figure 2012100746408100002DEST_PATH_IMAGE016
, sampling when the medial temperature
Figure 2012100746408100002DEST_PATH_IMAGE018
of coal gas, sampling, sampling and t ℃ is calculated as follows and obtains
Figure 910519DEST_PATH_IMAGE002
:
Figure 2012100746408100002DEST_PATH_IMAGE024
In the formula:
Figure 819831DEST_PATH_IMAGE016
---sample volume shown in the wet test meter, L;
Figure 2012100746408100002DEST_PATH_IMAGE026
---the correction coefficient of wet test meter;
Figure 298086DEST_PATH_IMAGE018
---the medial temperature of coal gas during sampling, ℃;
Figure 502802DEST_PATH_IMAGE020
---the atmospheric pressure during sampling, kPa;
Figure 387188DEST_PATH_IMAGE022
---the gas pressure during sampling, kPa;
Saturation vapor pressure in the time of W---t ℃, kPa.
The coal gas of said step (1) be feed successively two be equipped with potassium hydroxide solution the bottle in; When reaching the gas sampling volume for
Figure 993750DEST_PATH_IMAGE002
; Two bottles of absorption liquids are merged, must be absorbed with the sample absorption liquid of hydrogen cyanide.
The present invention adopts potassium hydroxide solution to absorb the hydrogen cyanide in the coal gas, transfers to absorption liquid in the volumetric flask of certain volume, gets a certain amount of absorption liquid; Add cadmium acetate solution, make the sulfide in the absorption liquid form the indissoluble sulfide-cadmium precipitation, after filtering, washing; Can remove sediment; Filtrating is made indicator with p-dimethylaminobenzal rhodanine, uses the silver nitrate standard solution titration, and cryanide ion and silver nitrate effect form silver soluble cyanogen complex ion (Ag (CN) 2), excessive silver ion and p-dimethylaminobenzal rhodanine indicator reaction, it is orange red that solution is become by yellow, is terminal point, according to the volume calculation hydrogen cyanide content of the silver nitrate standard solution that consumes.
The invention solves the plurality of reagents poisonous and harmful that uses in the prior art, analytical procedure is complicated, length consuming time, and there is potential safety hazard in the mensuration process, increases problems such as back segment wastewater treatment load, can fast, accurately measure the content of hydrogen cyanide in the coke-oven gas.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
(1) in two bottle that the potassium hydroxide solution that mass concentration is 30%, volume is 50mL is housed respectively; Feed coal gas to gas sampling volume
Figure 174065DEST_PATH_IMAGE002
successively; Merge two bottles of absorption liquids, must be absorbed with the sample absorption liquid 100mL of hydrogen cyanide; Wherein, gas sampling volume passes through computes:
Figure 291505DEST_PATH_IMAGE024
Gas sampling volume
Figure 752573DEST_PATH_IMAGE016
is to measure with conventional wet test meter; Occurrence is that the correction coefficient
Figure 838210DEST_PATH_IMAGE026
of 110L (behind the tower), wet test meter is 0.91, the medial temperature
Figure 17518DEST_PATH_IMAGE018
of coal gas is 11.0 ℃ during sampling, the gas pressure
Figure 571000DEST_PATH_IMAGE022
of the atmospheric pressure
Figure 989846DEST_PATH_IMAGE020
during sampling during for 81.22KPa, sampling be 0 KPa; And the saturation vapor pressure W t ℃ the time is 1.303 KPa, and calculating gained
Figure 93117DEST_PATH_IMAGE002
is 80.05L:
(2) step (1) gained sample absorption liquid is diluted with water to 250mL; Shake up the sample dilution; Get this sample dilution of 10.00mL; And drip no yellow sulfide-cadmium precipitation in the clear liquid of cadmium acetate solution to upper strata therein, and excessive till produce a small amount of white precipitate, make the sulfide in the sample absorption liquid form indissoluble sulfide-cadmium precipitation thing and get into lower floor; After the filtration; With distilled water cyclic washing sediment, to 100mL, in sample filtrating, add 3 of p-dimethylaminobenzal rhodanine indicator then until the sample filtrate volume of collecting; Be yellow filtrating to orange red with the silver nitrate standard solution titration, the volume that obtains the silver nitrate standard solution that titration sample filtrating consumed is 1.00mL for ;
(3) get 80mL water; And in water, to add the 4mL mass concentration be potassium hydroxide solution and 2 cadmium acetate solution of 30%; Add 3 p-dimethylaminobenzal rhodanine indicator again; The blank solution that shakes up yellowly; With the silver nitrate standard solution titration should yellow blank solution to orange red, the volume that obtains the silver nitrate standard solution that the titration blank solution consumes is 0.04mL for
Figure 526952DEST_PATH_IMAGE006
;
(4) content through hydrogen cyanide in the computes coke-oven gas is 0.32g/m 3:
In the formula:
Figure 265418DEST_PATH_IMAGE010
---the quality of suitable with 1.00mL silver nitrate standard solution (1.000 mol/L) hydrogen cyanide with the gram expression;
Figure 403007DEST_PATH_IMAGE012
---the concentration of silver nitrate standard solution, 0.0198mol/L;
Figure 223196DEST_PATH_IMAGE004
---the volume of the silver nitrate standard solution that titration sample filtrating is consumed, 1.00mL;
Figure 261165DEST_PATH_IMAGE014
---the volume of the silver nitrate standard solution that the titration blank solution is consumed, 0.04mL;
Figure 141397DEST_PATH_IMAGE002
---be scaled 101.325KPa, the gas sampling volume 15 ℃ the time, 80.05L.
Embodiment 2
(1) in two bottle that the potassium hydroxide solution that mass concentration is 35%, volume is 60mL is housed respectively; Feed coal gas to gas sampling volume
Figure 766282DEST_PATH_IMAGE002
successively; Merge two bottles of absorption liquids, must be absorbed with the sample absorption liquid of hydrogen cyanide; Wherein, gas sampling volume
Figure 124582DEST_PATH_IMAGE002
passes through computes:
Figure 285567DEST_PATH_IMAGE024
Gas sampling volume
Figure 805541DEST_PATH_IMAGE016
is to measure with conventional wet test meter; Occurrence is that the correction coefficient
Figure 917723DEST_PATH_IMAGE026
of 100L (behind the tower), wet test meter is 0.91, the medial temperature
Figure 79714DEST_PATH_IMAGE018
of coal gas is 6 ℃ during sampling, the saturation vapor pressure W the when gas pressure
Figure 48730DEST_PATH_IMAGE022
the when atmospheric pressure
Figure 826697DEST_PATH_IMAGE020
during sampling is 81.53 KPa, sampling is 0 KPa and t ℃ is 0.935 KPa, and calculating gained
Figure 992416DEST_PATH_IMAGE002
is 74.73 L:
(2) step (1) gained sample absorption liquid is diluted with water to 250mL; Shake up the sample dilution; Get this sample dilution of 10.00mL; And drip no yellow sulfide-cadmium precipitation in the clear liquid of cadmium acetate solution to upper strata therein, and excessive till produce a small amount of white precipitate, make the sulfide in the sample absorption liquid form indissoluble sulfide-cadmium precipitation thing and get into lower floor; After the filtration; With distilled water cyclic washing sediment, to 100mL, in sample filtrating, add 3 of p-dimethylaminobenzal rhodanine indicator then until the sample filtrate volume of collecting; Be yellow filtrating to orange red with the silver nitrate standard solution titration, the volume that obtains the silver nitrate standard solution that titration sample filtrating consumed is 0.86mL for
Figure 207365DEST_PATH_IMAGE004
;
(3) get 80mL water; And in water, to add the 4mL mass concentration be potassium hydroxide solution and 2 cadmium acetate solution of 35%; Add 3 p-dimethylaminobenzal rhodanine indicator again; The blank solution that shakes up yellowly; With the silver nitrate standard solution titration should yellow blank solution to orange red, the volume that obtains the silver nitrate standard solution that the titration blank solution consumes is 0.04mL for
Figure 326631DEST_PATH_IMAGE006
;
(4) content through hydrogen cyanide in the computes coke-oven gas is 0.29 g/m 3:
Figure 204719DEST_PATH_IMAGE008
In the formula:
Figure 42225DEST_PATH_IMAGE010
---the quality of suitable with 1.00mL silver nitrate standard solution (1.000 mol/L) hydrogen cyanide with the gram expression;
Figure 795287DEST_PATH_IMAGE012
---the concentration of silver nitrate standard solution, 0.0198mol/L;
---the volume of the silver nitrate standard solution that titration sample filtrating is consumed, 0.86mL mL;
---the volume of the silver nitrate standard solution that the titration blank solution is consumed, 0.04mL mL;
Figure 405500DEST_PATH_IMAGE002
---be scaled 101.325KPa, the gas sampling volume 15 ℃ the time is 74.73 L.
Embodiment 3
(1) in two bottle that the potassium hydroxide solution that mass concentration is 40%, volume is 55mL is housed respectively; Feed coal gas to gas sampling volume
Figure 368777DEST_PATH_IMAGE002
, must be absorbed with the sample absorption liquid of hydrogen cyanide; Wherein, gas sampling volume
Figure 947788DEST_PATH_IMAGE002
passes through computes:
Figure 682526DEST_PATH_IMAGE024
Wherein, Gas sampling volume
Figure 478313DEST_PATH_IMAGE016
is to measure with conventional wet test meter; Occurrence is that the correction coefficient
Figure 589488DEST_PATH_IMAGE026
of 60L (before the tower), wet test meter is 0.92, the medial temperature
Figure 297374DEST_PATH_IMAGE018
of coal gas is 10 ℃ during sampling, the saturation vapor pressure W the when gas pressure
Figure 830303DEST_PATH_IMAGE022
the when atmospheric pressure
Figure 796488DEST_PATH_IMAGE020
during sampling is 81.20 KPa, sampling is 0 KPa and t ℃ is 1.228 KPa, and calculating gained
Figure 728858DEST_PATH_IMAGE002
is 44.34L:
(2) step (1) gained sample absorption liquid is diluted with water to 250mL; Shake up the sample dilution; Get this sample dilution of 10.00mL; And drip no yellow sulfide-cadmium precipitation in the clear liquid of cadmium acetate solution to upper strata therein, and excessive till produce a small amount of white precipitate, make the sulfide in the sample absorption liquid form indissoluble sulfide-cadmium precipitation thing and get into lower floor; After the filtration; With distilled water cyclic washing sediment, to 100mL, in sample filtrating, add 3 of p-dimethylaminobenzal rhodanine indicator then until the sample filtrate volume of collecting; Be yellow filtrating to orange red with the silver nitrate standard solution titration, the volume that obtains the silver nitrate standard solution that titration sample filtrating consumed is 1.28mL;
(3) get 80mL water; And in water, to add the 4mL mass concentration be potassium hydroxide solution and 2 cadmium acetate solution of 40%; Add 3 p-dimethylaminobenzal rhodanine indicator again; The blank solution that shakes up yellowly; With the silver nitrate standard solution titration should yellow blank solution to orange red, the volume that obtains the silver nitrate standard solution that the titration blank solution consumes is 0.04mL for
Figure 359002DEST_PATH_IMAGE006
;
(4) content through hydrogen cyanide in the computes coke-oven gas is 0.75 g/m 3:
Figure 880113DEST_PATH_IMAGE008
In the formula:
Figure 316780DEST_PATH_IMAGE010
---the quality of suitable with 1.00mL silver nitrate standard solution (1.000 mol/L) hydrogen cyanide with the gram expression;
Figure 239736DEST_PATH_IMAGE012
---the concentration of silver nitrate standard solution, 0.0198mol/L;
Figure 234981DEST_PATH_IMAGE004
---the volume of the silver nitrate standard solution that titration sample filtrating is consumed, 1.28mL;
Figure 243388DEST_PATH_IMAGE014
---the volume of the silver nitrate standard solution that the titration blank solution is consumed, 0.04mL;
Figure 483745DEST_PATH_IMAGE002
---be scaled 101.325KPa, the gas sampling volume 15 ℃ the time, 44.34L.

Claims (2)

1. the assay method of hydrogen cyanide content in the coal gas is characterized in that through following each step:
(1) volume is
Figure 2012100746408100001DEST_PATH_IMAGE002
to feed coal gas to gas sampling in the potassium hydroxide solution that be 30～40% in mass concentration, volume is 100～120mL, must be absorbed with the sample absorption liquid of hydrogen cyanide;
(2) step (1) gained sample absorption liquid is diluted with water to 250mL; Shake up the sample dilution; Get this sample dilution 10mL; And drip no yellow sulfide-cadmium precipitation in the clear liquid of cadmium acetate solution to upper strata therein, and excessive till produce a small amount of white precipitate, make the sulfide in the sample absorption liquid form the sulfide-cadmium precipitation thing of indissoluble and get into lower floor; After the filtration; With distilled water cyclic washing sediment, to 100mL, in sample filtrating, add 3 of p-dimethylaminobenzal rhodanine indicator then until the sample filtrate volume of collecting; With silver nitrate standard solution titration sample filtrating to orange red, obtain silver nitrate standard solution that titration sample filtrating consumed volume is
Figure 2012100746408100001DEST_PATH_IMAGE004
;
(3) get 80mL water; And in water, to add the 4mL mass concentration be potassium hydroxide solution and 2 cadmium acetate solution of 30～40%; Add 3 p-dimethylaminobenzal rhodanine indicator again; The blank solution that shakes up yellowly; With the silver nitrate standard solution titration should yellow blank solution to orange red, obtain silver nitrate standard solution that the titration blank solution consumes volume is
Figure 2012100746408100001DEST_PATH_IMAGE006
;
(4) content through hydrogen cyanide in the computes coke-oven gas:
Figure 2012100746408100001DEST_PATH_IMAGE008
In the formula:
Figure 2012100746408100001DEST_PATH_IMAGE010
---the quality of suitable with 1.00mL silver nitrate standard solution (1.000 mol/L) hydrogen cyanide with the gram expression;
Figure 2012100746408100001DEST_PATH_IMAGE012
---the concentration of silver nitrate standard solution, mol/L;
Figure 150720DEST_PATH_IMAGE004
---the volume of the silver nitrate standard solution that titration sample filtrating is consumed, mL;
Figure 2012100746408100001DEST_PATH_IMAGE014
---the volume of the silver nitrate standard solution that the titration blank solution is consumed, mL;
Figure 788637DEST_PATH_IMAGE002
---be scaled 101.325KPa, the gas sampling volume 15 ℃ the time, L.
2. assay method according to claim 1; It is characterized in that: the gas sampling volume in the said step (1) is: the saturation vapor pressure W the when gas pressure
Figure 2012100746408100001DEST_PATH_IMAGE022
the when atmospheric pressure
Figure 2012100746408100001DEST_PATH_IMAGE020
during with conventional wet test meter metering sample volume
Figure 2012100746408100001DEST_PATH_IMAGE016
, sampling when the medial temperature
Figure 2012100746408100001DEST_PATH_IMAGE018
of coal gas, sampling, sampling and t ℃ is calculated as follows and obtains
Figure 822330DEST_PATH_IMAGE002
:
Figure 2012100746408100001DEST_PATH_IMAGE024
In the formula:
Figure 549240DEST_PATH_IMAGE016
---sample volume shown in the wet test meter, L;
---the correction coefficient of wet test meter;
Figure 918911DEST_PATH_IMAGE018
---the medial temperature of coal gas during sampling, ℃;
Figure 901910DEST_PATH_IMAGE020
---the atmospheric pressure during sampling, kPa;
Figure 982605DEST_PATH_IMAGE022
---the gas pressure during sampling, kPa;
Saturation vapor pressure in the time of W---t ℃, kPa.
CN2012100746408A 2012-03-21 2012-03-21 Method for testing content of hydrogen cyanide in gas Pending CN102636616A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN103234957A (en) * 2013-05-13 2013-08-07 浙江中一检测研究院股份有限公司 Method for determining concentration of cyanides in environment
CN103293151A (en) * 2013-06-11 2013-09-11 鞍钢股份有限公司 Method for detecting hydrogen sulfide, carbon dioxide and hydrogen cyanide in acid gas
CN103852509A (en) * 2014-03-19 2014-06-11 北京矿冶研究总院 Potentiometric titration analysis method for cyanide
CN104990827A (en) * 2015-06-15 2015-10-21 北京科技大学 Determining method and device for adsorption quantity of low-volatility organic gas on adsorbing materials
CN110470789A (en) * 2019-08-26 2019-11-19 四川达兴能源股份有限公司 The measuring method of hydrogen cyanide in a kind of coke-stove gas
CN114397400A (en) * 2021-12-06 2022-04-26 宜宾光原锂电材料有限公司 Method for determining content of nickel and cobalt in nickel and cobalt mixed salt

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103234957A (en) * 2013-05-13 2013-08-07 浙江中一检测研究院股份有限公司 Method for determining concentration of cyanides in environment
CN103234957B (en) * 2013-05-13 2015-04-15 浙江中一检测研究院股份有限公司 Method for determining concentration of cyanides in environment
CN103293151A (en) * 2013-06-11 2013-09-11 鞍钢股份有限公司 Method for detecting hydrogen sulfide, carbon dioxide and hydrogen cyanide in acid gas
CN103852509A (en) * 2014-03-19 2014-06-11 北京矿冶研究总院 Potentiometric titration analysis method for cyanide
CN103852509B (en) * 2014-03-19 2016-05-25 北京矿冶研究总院 Potentiometric titration analysis method for cyanide
CN104990827A (en) * 2015-06-15 2015-10-21 北京科技大学 Determining method and device for adsorption quantity of low-volatility organic gas on adsorbing materials
CN110470789A (en) * 2019-08-26 2019-11-19 四川达兴能源股份有限公司 The measuring method of hydrogen cyanide in a kind of coke-stove gas
CN110470789B (en) * 2019-08-26 2022-07-05 四川达兴能源股份有限公司 Method for determining hydrogen cyanide in coke oven gas
CN114397400A (en) * 2021-12-06 2022-04-26 宜宾光原锂电材料有限公司 Method for determining content of nickel and cobalt in nickel and cobalt mixed salt
CN114397400B (en) * 2021-12-06 2024-03-26 宜宾光原锂电材料有限公司 Method for measuring nickel and cobalt content in nickel and cobalt mixed salt

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Application publication date: 20120815