CN101672790A - Quick detecting tube for micro-hydrogen sulfide gas - Google Patents
Quick detecting tube for micro-hydrogen sulfide gas Download PDFInfo
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- CN101672790A CN101672790A CN200910093542A CN200910093542A CN101672790A CN 101672790 A CN101672790 A CN 101672790A CN 200910093542 A CN200910093542 A CN 200910093542A CN 200910093542 A CN200910093542 A CN 200910093542A CN 101672790 A CN101672790 A CN 101672790A
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Abstract
The invention relates to a detecting tube for low concentration hydrogen sulfide gas. Barium sulfate, silica gel or a mixture of the barium sulfate and the silica gel is used as a carrier; lead acetate solution and barium chloride solution are used as developing agents; glycerine is used as a wetting agent; and different detection indicators are obtained by controlling the dry condition. The hydrogen sulphide gas samples with different concentrations are introduced into the detecting tube, and the content of the hydrogen sulfide gas is determined according to the difference of the color changeof the developing agents. The detecting tube has simple structure, fast analysis, low cost and convenient carrying, and can detect weather the content of hydrogen sulfide in air of environment is over-proof at the field. The application experiment proves that the detecting tube has higher sensitivity and substantially meets the requirements of national standard.
Description
Technical field
The present invention relates to a kind of development of micro-hydrogen sulfide gas detector tube, comprise choosing of carrier and indicator, the carrier that is adsorbed with indicator is carried out the processing of different degree of dryings, and the control of sample size.
Background technology
Sulfuretted hydrogen is a kind of colourless, hypertoxic, highly acid gas.Sulfuretted hydrogen is mainly derived from a plurality of production runes such as iron and steel, oil refining, papermaking, fuel, pharmacy, process hides, also often comes across places such as methane-generating pit, colliery, oil well, sewer, cesspool.The toxicity of sulfuretted hydrogen is only second to prussiate, is easy causing death's toxic gas.Sulfuretted hydrogen not only serious threat people's life security, but also causes serious environmental to pollute, and hardware is caused serious corrosion failure.Simultaneously, sulfuretted hydrogen is the important source material of refining sulphur, is the precious resources of national defence and chemical industry.Therefore, for guaranteeing being perfectly safe of personnel, stop the generation of hydrogen sulfide poisoning accident, understand the source and the harm of hydrogen sulfide gas, the prevention of grasping hydrogen sulfide gas is extremely important with processing knowledge and sulfuretted hydrogen detection method.
Detection method to hydrogen sulfide gas has a lot, mainly contains standard iodimetric titration, methylene blue laws, vapor-phase chromatography, lead acetate reaction rate method, detector tube colourimetry etc.
The major defect of iodimetric titration is longer for the sulfuretted hydrogen sampling time of low content, and as the sample for the ppb order of magnitude, may reach 60min sample time; The methylene blue laws is only comparatively suitable to the more stable purified natural gas of concentration of hydrogen sulfide; Vapor-phase chromatography mainly is that detecting device, standard gas and sampling technique are had higher requirement; Lead acetate reaction rate method will adopt instrumentation to detect sulfuretted hydrogen.These assay methods, a shortcoming is all arranged: just be to use the equipment price height, bulky, need the energy, many times can not measure on the spot, go back to the laboratory again after all needing initiatively to sample earlier and analyze, prolong analysis time, increased analytical error, especially for the not high gas of stability.And the detector tube colourimetry is a kind of detection method more fast, and detector tube is easy to carry, and whether the content that can carry out sulfuretted hydrogen in the surrounding air at the scene exceeds standard.The effect of detector tube colourimetry is similar to the pH test paper, mainly is to the less demanding occasion of accuracy.
Summary of the invention
Technical matters to be solved by this invention is at above-mentioned deficiency of the prior art, and a kind of detector tube that can carry out fast measuring to low concentration hydrogen sulphide gas is provided.The invention provides silica gel or BaSO
4Or both potpourris are as carrier, and indicator is the mixed liquor of lead acetate solution or lead acetate and barium chloride.To the carrier drying that is adsorbed with indicator or moist or, in the glass tube of packing into, low concentration hydrogen sulphide gas sample is detected with the absolute ethyl alcohol dehydration.
Concrete grammar is as follows:
A. the preparation of carrier:
It is that 3.18 water glass and deionized water dilute with 1: 4～1: 8 volume ratio that the certain volume modulus is measured in the preparation of silica gel, uses the sulfuric acid titration, forms gel.By the consumption of control sulfuric acid, form the gel of pH=7～11.Gel washes with deionized water wash to pH=7 with a large amount of tap water earlier again, does not have SO in the filtrate
4 2-Exist.Suction filtration places the dry 1～4h of 100～200 ℃ of constant temperature ovens, and it is stand-by to make silica gel.
The preparation of barium sulphate takes by weighing the barium chloride of certain mass, is dissolved in the deionized water, and being mixed with concentration is 0.2～2.0mol/L barium chloride solution, adds sulfuric acid to not precipitation generation, stirs 10～60min, does not have SO with deionized water wash to filtrate
4 2-Exist.Suction filtration places the dry 1～4h of 100～200 ℃ of constant temperature ovens, makes BaSO
4Stand-by.
B. the preparation of adsorption indicator:
The preparation of carrier absorption lead acetate indicator joins 5～15mL glycerine in the lead acetate solution that 10～50mL concentration is 0.1～0.5mol/L, mix, 2～10g carrier is added in the mixed liquor, stirring makes it abundant mixing, at room temperature 10～24h is placed in the dark place, suction filtration, the control drying condition.
It is in the mixed liquor of the lead acetate solution of 0.1～0.5mol/L and the barium chloride solution that 10～50mL concentration is 0.1～0.5mol/L to concentration that the preparation of carrier absorption lead acetate and barium chloride indicator adds 10～50mL with 5～15mL glycerine, mix, 2～10g carrier is added in the mixed liquor, stirring makes it abundant mixing, at room temperature 10～24h is placed in the dark place, suction filtration, the control drying condition.
C. the preparation of detector tube: the carrier that will be adsorbed with indicator 6 diameters of packing into are in the glass tube of 4mm, and label, make H
2The S gas detecting tube.
D. the preparation of stink damp sample: with FeS and rare H
2SO
4Reaction makes, and extracts the pure H of different volumes respectively with syringe (volume is 5mL)
2S mixes with a certain proportion of a large amount of air, is made into volume fraction and is 0.000%, 0.001%, 0.002%, 0.004%, 0.006% and 0.008% H
2S gas sample is demarcated concentration with vapor-phase chromatography.
E. the detection of sulfuretted hydrogen: the H that draws variable concentrations with syringe
2S gas injects each detector tube respectively, and throughput is 50mL, and duration of ventilation is 1min.According to each detector tube change color difference, can make standard colorimetric strake.
Compared with prior art, the present invention has following characteristics:
Better effects if when (1) micro-hydrogen sulfide gas detector tube of the present invention adopts barium sulphate to make carrier.
(2) micro-hydrogen sulfide gas detector tube of the present invention adopts barium sulphate absorption lead acetate and barium chloride mixed liquor as indicator, in the presence of barium chloride, there is the part lead acetate to change into lead chloride, promoted plumbous deposition, help the absorption of barium sulphate to lead, increase the concentration of barium sulphate surface adsorption lead, improved the sensitivity that detects.
(3) micro-hydrogen sulfide gas detector tube of the present invention has been controlled suitable drying condition, can reduce the carrier surface moisture to the carrier that is adsorbed with indicator with absolute ethanol washing, moist, can guarantee the humidity that carrier surface is suitable, can improve the sensitivity of detection.
(4) the low concentration hydrogen sulphide gas detecting tube sampling time of the present invention is short, sample size is few.The throughput of relevant fast measuring pipe method bibliographical information is all bigger, adopts the gas production bag of 1.0L usually.And detector tube throughput of the present invention only is 50mL, has improved detection sensitivity.
(5) low concentration hydrogen sulphide gas detecting tube of the present invention easy, quick, be easy to carry, highly sensitive and cheap, selected indicator is easy to get, environmental pollution is little.Can be at the scene whether the content of sulfuretted hydrogen in the surrounding air being exceeded standard and detect, mainly is to be used for the less demanding occasion of accuracy.
Embodiment
Embodiment 1:
Measure modulus and be 3.18 water glass 75mL, add deionized water 300mL, stir 10min.Use the sulfuric acid titration, form pH of latex gel=8, gel washes with deionized water wash to pH=7 with a large amount of tap water earlier again, does not have SO in the filtrate
4 2-Exist.Suction filtration places 120 ℃ of dry 2h of constant temperature oven, makes silica gel.Weighing 2gPb (Ac)
23H
2O is dissolved in the 20mL deionized water, adds glycerine 10mL, mixes, and 5g silica gel is added in the mixed liquor, stirs and makes it abundant mixing, and at room temperature 16h is placed in the dark place, suction filtration, dry 1h under 60 ℃ in constant temperature oven.With the carrier that is adsorbed with indicator 6 diameters of packing into is in the glass tube of 4mm, and label, feeds volume fraction respectively and be 0.000%, 0.001%, 0.002%, 0.004%, 0.006% and 0.008% H
2S gas sample.Sample size is 50mL, and duration of ventilation is 1min.Experimental result shows that when the feeding volume fraction was 0.006% and 0.008% gas sample, detector tube had significant change color, therefore, detects and is limited to 0.006%, is about 90mg/m
3
Embodiment 2:
With embodiment 1 contrast, change indicator and drying condition.Weighing 2gPb (Ac)
23H
2O and 1gBaCl
22H
2O is dissolved in respectively in the 20mL deionized water, and lead acetate solution and barium chloride solution are mixed, and adds glycerine 10mL, mixes, and 5g silica gel is added in the mixed liquor, stirs and makes it abundant mixing, and at room temperature 16h, suction filtration are placed in the dark place.With the carrier that is adsorbed with indicator 6 diameters of packing into is in the glass tube of 4mm, and label, feeds volume fraction respectively and be 0.000%, 0.001%, 0.002%, 0.004%, 0.006% and 0.008% H
2S gas sample.Sample size is 50mL, and duration of ventilation is 1min.Experimental result shows, is 0.004% and during the gas sample of higher concentration when feeding volume fraction, and detector tube has significant change color, detects and is limited to 0.004%, is about 60mg/m
3
Embodiment 3:
Weighing 30gBaCl
22H
2O is dissolved in the 100mL deionized water, adds sulfuric acid to not precipitation generation, stirs 30min, does not have SO with deionized water wash to filtrate
4 2-Exist.Suction filtration places 120 ℃ of dry 2h of constant temperature oven, makes BaSO
4Weighing 2gPb (Ac)
23H
2O is dissolved in the 20mL deionized water, adds glycerine 10mL, mixes, with 5g BaSO
4Add in the mixed liquor, stir and make it abundant mixing, at room temperature 16h is placed in the dark place, suction filtration, dry 1h under 60 ℃ in constant temperature oven.With the carrier that is adsorbed with indicator 6 diameters of packing into is in the glass tube of 4mm, and label, feeds volume fraction respectively and be 0.000%, 0.001%, 0.002%, 0.004%, 0.006% and 0.008% H
2S gas sample.Sample size is 50mL, and duration of ventilation is 1min.Experimental result shows, is 0.004% and during the gas sample of higher concentration when feeding volume fraction, and detector tube has significant change color, detects and is limited to 0.004%, is about 60mg/m
3
Embodiment 4:
With embodiment 3 contrasts, change indicator and drying condition.Weighing 2gPb (Ac)
23H
2O and 1gBaCl
22H
2O is dissolved in respectively in the 20mL deionized water, and lead acetate solution and barium chloride solution are mixed, and adds 10mL glycerine, with 5g BaSO
4Add in the mixed liquor, stir and make it abundant mixing, at room temperature 16h, suction filtration are placed in the dark place.With the carrier that is adsorbed with indicator 6 diameters of packing into is in the glass tube of 4mm, and label, feeds volume fraction respectively and be 0.000%, 0.001%, 0.002%, 0.004%, 0.006% and 0.008% H
2S gas sample.Sample size is 50mL, and duration of ventilation is 1min.。Experimental result shows, is 0.002% and during the gas sample of higher concentration when feeding volume fraction, and detector tube has significant change color, detects and is limited to 0.002%, is about 30mg/m
3
Embodiment 5
With embodiment 4 contrasts, change concentration of indicator and drying condition.Weighing 4gPb (Ac)
23H
2O and 2gBaCl
22H
2O is dissolved in respectively in the 20mL deionized water, and lead acetate solution and barium chloride solution are mixed, and adds 10mL glycerine, with 5g BaSO
4Add in the mixed liquor, stir and make it abundant mixing, at room temperature 16h is placed in the dark place, uses absolute ethanol washing, suction filtration.With the carrier that is adsorbed with indicator 6 diameters of packing into is in the glass tube of 4mm, and label, feeds volume fraction respectively and be 0.000%, 0.001%, 0.002%, 0.004%, 0.006% and 0.008% H
2S gas sample.Sample size is 50mL, and duration of ventilation is 1min.Experimental result shows, is 0.001% and during the gas sample of higher concentration when feeding volume fraction, and detector tube has significant change color, detects and is limited to 0.001%, is about 15mg/m
3
Embodiment 6
Silica gel and barium sulphate potpourri are as carrier.Weighing 4gPb (Ac)
23H
2O and 2gBaCl
22H
2O is dissolved in respectively in the 20mL deionized water, and lead acetate solution and barium chloride solution are mixed, and adds 10mL glycerine, with 5g silica gel and 5g BaSO
4Add in the mixed liquor, stir and make it abundant mixing, at room temperature 16h is placed in the dark place, uses absolute ethanol washing, suction filtration.With the carrier that is adsorbed with indicator 6 diameters of packing into is in the glass tube of 4mm, and label, feeds volume fraction respectively and be 0.000%, 0.001%, 0.002%, 0.004%, 0.006% and 0.008% H
2S gas sample.Sample size is 50mL, and duration of ventilation is 1min.Experimental result shows, is 0.002% and during the gas sample of higher concentration when feeding volume fraction, and detector tube has significant change color, detects and is limited to 0.002%, is about 30mg/m
3
Claims (6)
1. a quick detecting tube for micro-hydrogen sulfide gas is characterized in that, dress is adsorbed with the carrier of gas detection indicator in the body.Carrier is silica gel or barium sulphate or both potpourris; Indicator is lead acetate solution or the lead acetate of carrier surface absorption and the mixed liquor of barium chloride of carrier surface absorption; The carrier adsorption indicator also adds after glycerine makes wetting agent, obtains different H
2The S gas detecting tube.
2. quick detecting tube for micro-hydrogen sulfide gas according to claim 1, it is characterized in that, modulus is 2.0～3.2 water glass and deionized water with 1: 4～1: 8 volume ratio dilution, form pH=7～11 gels with the sulfuric acid titration, washing, suction filtration, at 100～200 ℃ of down dry 1～4h, the silica gel of pH=7.
3. quick detecting tube for micro-hydrogen sulfide gas according to claim 1, it is characterized in that concentration is to add sulfuric acid to precipitation in the barium chloride solution of 0.2～2.0mol/L to generate, and stirs 10～60min, with deionized water wash, suction filtration, at 100～200 ℃ of down dry 1～4h, barium sulphate.
4. quick detecting tube for micro-hydrogen sulfide gas according to claim 1, it is characterized in that, 5～15mL glycerine is joined in the lead acetate solution that 10～50mL concentration is 0.1～0.5mol/L, 2～10g carrier is joined in this mixed liquor after 10～24h is placed in the dark place under the room temperature, make carrier surface absorption lead acetate indicator.
5. quick detecting tube for micro-hydrogen sulfide gas according to claim 1, it is characterized in that, 5～15mL glycerine is joined in the mixed liquor of the barium chloride solution that lead acetate solution that 10～50mL concentration is 0.1～0.5mol/L and 10～50mL concentration is 0.1～0.5mol/L, 2～10g carrier is joined in this mixed liquor after 10～24h is placed in the dark place under the room temperature, make carrier surface absorption lead acetate and barium chloride indicator.
6. pipe is surveyed in micro-hydrogen sulfide gas according to claim 1 inspection fast, it is characterized in that, the carrier adsorption indicator also adds glycerine and does to carry out drying or use absolute ethanol washing behind the wetting agent, and baking temperature is no more than 75 ℃, is no more than 2h drying time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910093542A CN101672790A (en) | 2009-10-13 | 2009-10-13 | Quick detecting tube for micro-hydrogen sulfide gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910093542A CN101672790A (en) | 2009-10-13 | 2009-10-13 | Quick detecting tube for micro-hydrogen sulfide gas |
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| CN101672790A true CN101672790A (en) | 2010-03-17 |
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ID=42020110
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|---|---|---|---|
| CN200910093542A Pending CN101672790A (en) | 2009-10-13 | 2009-10-13 | Quick detecting tube for micro-hydrogen sulfide gas |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128797A (en) * | 2010-12-09 | 2011-07-20 | 湖北兴发化工集团股份有限公司 | Method for measuring total sulfur content in yellow phosphorus tail gas |
| CN102507578A (en) * | 2011-11-01 | 2012-06-20 | 中国石油大学(华东) | Instrument for on-line monitoring hydrogen sulfide in drilling fluid |
| CN102721686A (en) * | 2012-06-20 | 2012-10-10 | 中华人民共和国盐城出入境检验检疫局 | Method for detecting harmful gases generated by burning of fireworks and firecrackers |
| CN102854161A (en) * | 2012-09-07 | 2013-01-02 | 江苏南瓷绝缘子有限公司 | Test method for hydrogen sulfide concentration |
| CN103969261A (en) * | 2014-05-12 | 2014-08-06 | 内蒙古工业大学 | Method for measuring sulfur content of steppe plant |
| CN104391080A (en) * | 2014-11-19 | 2015-03-04 | 苏州东辰林达检测技术有限公司 | Trace hydrogen sulfide detection reagent and preparation method thereof |
| CN104568940A (en) * | 2015-01-29 | 2015-04-29 | 国家纳米科学中心 | Method for detecting hydrogen sulfide gas based on nanocrystalline celluloses |
| CN107831267A (en) * | 2017-10-12 | 2018-03-23 | 中国海洋石油总公司 | A kind of liquid desulfurizing agent Lab-evaluation device and its evaluation method |
| CN108548787A (en) * | 2018-04-11 | 2018-09-18 | 黑龙江工程学院 | A kind of method that spectrometer accurately measures sulfureted hydrogen gas concentration |
| CN109825385A (en) * | 2018-12-29 | 2019-05-31 | 陈红 | A kind of urinal deodorization soap tablet prepared using citrus peel residue |
| CN112051258A (en) * | 2020-08-20 | 2020-12-08 | 北方华锦化学工业股份有限公司 | Method for analyzing whether residues in oil refining device pipeline/equipment contain ferrous sulfide |
| CN112505030A (en) * | 2020-12-03 | 2021-03-16 | 国网湖北省电力有限公司电力科学研究院 | For SF6SO in decomposition product gas2Component detection device and method |
| CN113189093A (en) * | 2021-04-28 | 2021-07-30 | 西南石油大学 | Method for detecting and monitoring hydrogen sulfide gas |
| CN114018913A (en) * | 2021-11-09 | 2022-02-08 | 河南省奥瑞环保科技股份有限公司 | Rapid gas detection tube carrier pretreatment method |
| CN114088694A (en) * | 2021-10-21 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Method for rapidly determining content of hydrogen sulfide in wastewater |
-
2009
- 2009-10-13 CN CN200910093542A patent/CN101672790A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128797A (en) * | 2010-12-09 | 2011-07-20 | 湖北兴发化工集团股份有限公司 | Method for measuring total sulfur content in yellow phosphorus tail gas |
| CN102507578A (en) * | 2011-11-01 | 2012-06-20 | 中国石油大学(华东) | Instrument for on-line monitoring hydrogen sulfide in drilling fluid |
| CN102507578B (en) * | 2011-11-01 | 2014-03-19 | 中国石油大学(华东) | Instrument for on-line monitoring hydrogen sulfide in drilling fluid |
| CN102721686A (en) * | 2012-06-20 | 2012-10-10 | 中华人民共和国盐城出入境检验检疫局 | Method for detecting harmful gases generated by burning of fireworks and firecrackers |
| CN102854161A (en) * | 2012-09-07 | 2013-01-02 | 江苏南瓷绝缘子有限公司 | Test method for hydrogen sulfide concentration |
| CN103969261A (en) * | 2014-05-12 | 2014-08-06 | 内蒙古工业大学 | Method for measuring sulfur content of steppe plant |
| CN104391080A (en) * | 2014-11-19 | 2015-03-04 | 苏州东辰林达检测技术有限公司 | Trace hydrogen sulfide detection reagent and preparation method thereof |
| CN104568940B (en) * | 2015-01-29 | 2017-02-22 | 国家纳米科学中心 | Method for detecting hydrogen sulfide gas based on nanocrystalline celluloses |
| CN104568940A (en) * | 2015-01-29 | 2015-04-29 | 国家纳米科学中心 | Method for detecting hydrogen sulfide gas based on nanocrystalline celluloses |
| CN107831267A (en) * | 2017-10-12 | 2018-03-23 | 中国海洋石油总公司 | A kind of liquid desulfurizing agent Lab-evaluation device and its evaluation method |
| CN108548787A (en) * | 2018-04-11 | 2018-09-18 | 黑龙江工程学院 | A kind of method that spectrometer accurately measures sulfureted hydrogen gas concentration |
| CN108548787B (en) * | 2018-04-11 | 2020-11-17 | 黑龙江工程学院 | Method for accurately measuring concentration of hydrogen sulfide gas by spectrometer |
| CN109825385A (en) * | 2018-12-29 | 2019-05-31 | 陈红 | A kind of urinal deodorization soap tablet prepared using citrus peel residue |
| CN112051258A (en) * | 2020-08-20 | 2020-12-08 | 北方华锦化学工业股份有限公司 | Method for analyzing whether residues in oil refining device pipeline/equipment contain ferrous sulfide |
| CN112505030A (en) * | 2020-12-03 | 2021-03-16 | 国网湖北省电力有限公司电力科学研究院 | For SF6SO in decomposition product gas2Component detection device and method |
| CN113189093A (en) * | 2021-04-28 | 2021-07-30 | 西南石油大学 | Method for detecting and monitoring hydrogen sulfide gas |
| CN114088694A (en) * | 2021-10-21 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Method for rapidly determining content of hydrogen sulfide in wastewater |
| CN114018913A (en) * | 2021-11-09 | 2022-02-08 | 河南省奥瑞环保科技股份有限公司 | Rapid gas detection tube carrier pretreatment method |
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Open date: 20100317 |