CN114544495A - Methylene blue spectrophotometry absorption liquid, preparation method thereof and determination method of hydrogen sulfide in sewage treatment station - Google Patents
Methylene blue spectrophotometry absorption liquid, preparation method thereof and determination method of hydrogen sulfide in sewage treatment station Download PDFInfo
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- CN114544495A CN114544495A CN202210142107.4A CN202210142107A CN114544495A CN 114544495 A CN114544495 A CN 114544495A CN 202210142107 A CN202210142107 A CN 202210142107A CN 114544495 A CN114544495 A CN 114544495A
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- methylene blue
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229960000907 methylthioninium chloride Drugs 0.000 title claims abstract description 45
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 38
- 238000002798 spectrophotometry method Methods 0.000 title claims abstract description 37
- 239000007788 liquid Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 22
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010865 sewage Substances 0.000 title claims abstract description 10
- 238000001514 detection method Methods 0.000 claims abstract description 7
- -1 sulfur ions Chemical class 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- SATHPVQTSSUFFW-UHFFFAOYSA-N 4-[6-[(3,5-dihydroxy-4-methoxyoxan-2-yl)oxymethyl]-3,5-dihydroxy-4-methoxyoxan-2-yl]oxy-2-(hydroxymethyl)-6-methyloxane-3,5-diol Chemical compound OC1C(OC)C(O)COC1OCC1C(O)C(OC)C(O)C(OC2C(C(CO)OC(C)C2O)O)O1 SATHPVQTSSUFFW-UHFFFAOYSA-N 0.000 claims description 6
- 229920000189 Arabinogalactan Polymers 0.000 claims description 6
- 239000001904 Arabinogalactan Substances 0.000 claims description 6
- 235000019312 arabinogalactan Nutrition 0.000 claims description 6
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 6
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000002912 waste gas Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims description 2
- 241000334160 Isatis Species 0.000 claims description 2
- BZORFPDSXLZWJF-UHFFFAOYSA-N N,N-dimethyl-1,4-phenylenediamine Chemical compound CN(C)C1=CC=C(N)C=C1 BZORFPDSXLZWJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 20
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 7
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a methylene blue spectrophotometry absorption liquid, a preparation method thereof and a determination method of hydrogen sulfide in a sewage treatment station, relating to the technical field of hydrogen sulfide detection, and comprising the following steps of S1: step S1: preparing methylene blue spectrophotometry absorption liquid; step S2; adding 3-5 drops of 10mmol/LEDTA solution into every 100mL of methylene blue spectrophotometry absorption liquid; step S3; adjusting the concentration of the absorption liquid. When in use, the problems of poor precision, poor stability and complex operation in the prior art are solved. And simultaneously conceals the interference of metal ions such as iron and the like on sulfur ions. The method has the advantages of simple and convenient operation, high precision and stability.
Description
Technical Field
The invention relates to the technical field of hydrogen sulfide detection, in particular to a methylene blue spectrophotometry absorption liquid, a preparation method thereof and a determination method of hydrogen sulfide in a sewage treatment station.
Background
The hydrogen sulfide is an inorganic compound, has a molecular formula of H2S and a molecular weight of 34.076, is a flammable acidic gas under standard conditions, is colorless, has a smelly egg smell at low concentration, has a sulfur smell at very low concentration, and is extremely toxic. The aqueous solution is hydrogen sulfuric acid, which is less acidic than carbonic acid, but more strongly boric acid. Can be dissolved in water and easily dissolved in alcohols, petroleum solvents and crude oil.
The methods for measuring the concentration of hydrogen sulfide in air provided by air and waste gas monitoring and analyzing method in the ministry of record and Commission of the State environmental protection administration include gas chromatography, methylene blue spectrophotometry and direct color-developing spectrophotometry.
The existing methylene blue spectrophotometry is a classical method, has the advantages of sensitivity, rapidness and the like, but has poor precision and stability and complicated operation. And the presence of metallic elements such as iron oxidizes sulfur ions.
Disclosure of Invention
The invention aims to provide a methylene blue spectrophotometry absorption liquid, a preparation method thereof and a determination method of hydrogen sulfide in a sewage treatment station, which are used for solving the technical problems.
The technical scheme adopted by the invention is as follows:
a preparation method of a novel methylene blue spectrophotometry absorption liquid comprises the following steps:
step S1: preparing methylene blue spectrophotometry absorption liquid;
step S2; adding 3-5 drops of 10mmol/L EDTA solution into every 100mL methylene blue spectrophotometry absorption liquid;
step S3; adjusting the concentration of the absorption liquid.
Further preferably, the step S1 includes weighing 4.3g of cadmium sulfate, 0.3g of sodium hydroxide and 10g of ammonium polyvinyl alcohol phosphate, respectively dissolving in a small amount of solvent dissolving solution, mixing the three solutions together, shaking vigorously, mixing well, and diluting to 1000mL with a solvent.
As a further preference, the solvent is water.
As a further preference, the step S1 includes weighing 4.3g of cadmium sulfate, 0.3g of sodium hydroxide and 10g of arabinogalactan, respectively dissolving in a small amount of solvent, mixing the three solutions together, shaking vigorously, mixing well, and diluting to 1000mL with solvent.
More preferably, the dissolving liquid is water.
A novel methylene blue spectrophotometry absorption liquid is prepared by the preparation method of any one of the novel methylene blue spectrophotometry absorption liquids.
A method for measuring hydrogen sulfide in a sewage treatment station is carried out by using a novel methylene blue spectrophotometry absorption liquid prepared by any one preparation method of the novel methylene blue spectrophotometry absorption liquid, and comprises the following steps:
step A, fully contacting the novel methylene blue spectrophotometry absorption liquid with waste gas of a sewage treatment station;
b, absorbing hydrogen sulfide in the waste gas by a novel methylene blue spectrophotometry absorption liquid to generate cadmium sulfide colloidal precipitate;
and step C, the sulfide ions and the p-aminodimethylaniline solution neutralize the ferric trichloride solution to generate methylene blue, and the methylene isatis root is observed according to the color depth and is measured by a spectrophotometry.
Further preferably, the methylene blue spectrophotometry detection limit is 0.07. mu.g/10 mL, and the lowest detection concentration is 0.001mg/m when the volume of the sampled exhaust gas is 60L3。
The technical scheme has the following advantages or beneficial effects:
based on the prior art, 3-5 drops of 10mmol/L EDTA solution are added into every 100mL of absorption liquid to improve the precision of sulfide on the basis of methylene blue spectrophotometry absorption liquid.
Compared with the prior art, the method saves the development cost of a new material, reduces the research and development time, and provides powerful support for the technical improvement and process optimization of products. The successful development of a new glass material requires strict material design and complex processing procedures.
The invention overcomes the problems of poor precision, poor stability and complex operation in the prior art. And simultaneously conceals the interference of metal ions such as iron and the like on sulfur ions. The method has the advantages of simple and convenient operation, high precision and stability.
Drawings
FIG. 1 is a graph comparing the results of 20 sets of experiments before and after addition of EDTA solution;
FIG. 2 is a graph comparing the stability of a hydrogen sulfide solution on standing;
FIG. 3 is a flow chart of the preparation method of the methylene blue spectrophotometry absorption liquid.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", and the like, which indicate orientations or positional relationships, are based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
Combining fig. 1 and fig. 3, in the first example, a novel methylene blue spectrophotometric absorption liquid was prepared.
Step S1: preparing methylene blue spectrophotometry absorption liquid, weighing 4.3g of cadmium sulfate, 0.3g of sodium hydroxide and 10g of ammonium polyvinyl alcohol phosphate, respectively dissolving in a small amount of solvent dissolving solution, mixing the three solutions together, strongly shaking, uniformly mixing, and diluting to 1000mL by using a solvent; step S2; adding 3-5 drops of 10mmol/L EDTA solution into every 100mL methylene blue spectrophotometry absorption solution; step S3; adjusting the concentration of the absorption liquid.
Example two, a novel methylene blue spectrophotometric absorption solution was prepared using arabinogalactan instead of ammonium polyvinyl alcohol phosphate.
Step S1: preparing methylene blue spectrophotometry absorption liquid, weighing 4.3g of cadmium sulfate, 0.3g of sodium hydroxide and 10g of arabinogalactan, respectively dissolving in a small amount of solvent, mixing the three solutions together, strongly shaking, uniformly mixing, and diluting to 1000mL by using the solvent; step S2; adding 3-5 drops of 10mmol/L EDTA solution into every 100mL methylene blue spectrophotometry absorption liquid; step S3; adjusting the concentration of the absorption liquid.
In the third embodiment, as can be seen from the data analysis in fig. 1, the relative standard deviation of the methylene blue spectrophotometry of the air and exhaust gas monitoring and analyzing method in the committee of the ministry of environmental protection, ministry of record of air and exhaust gas monitoring and analyzing method, at the 2 microgram concentration position, is about 2.61%, the relative standard deviation of the invention at the 2 microgram concentration position is about 1.96%, and the homologous ratio is reduced by about 0.65%, so that the invention can achieve the purpose of improving the stability.
In the fourth example, which can be analyzed from fig. 2, the time for storing the sulfide sample can be prolonged by at least 2 days after the arabinogalactan is added, so that the stability of the sulfide sample is greatly improved.
In the fifth example, based on the methylene blue spectrophotometric absorption solution of air and exhaust gas monitoring and analyzing method from the ministry of record and Commission of the State environmental protection agency of the State environmental protection, 3 to 5 drops of 10mmol/L EDTA solution were added to 100mL of the absorption solution. The EDTA solution can effectively conceal the oxidation effect of metal ions on sulfur ions. So that the precision of the detection of the invention is improved. On the basis, 2 micrograms of hydrogen sulfide samples are subjected to improved comparison; in addition, arabinogalactan is added into the absorption liquid to increase the stability of the sulfide in water, prolong the storage time of the sulfide and improve the stability.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A preparation method of novel methylene blue spectrophotometry absorption liquid is characterized by comprising the following steps:
step S1: preparing methylene blue spectrophotometry absorption liquid;
step S2; adding 3-5 drops of 10mmol/LEDTA solution into every 100mL of methylene blue spectrophotometry absorption liquid;
step S3; adjusting the concentration of the absorption liquid.
2. The method for preparing a novel methylene blue spectrophotometric absorbing solution as claimed in claim 1, wherein the step S1 comprises weighing 4.3g of cadmium sulfate, 0.3g of sodium hydroxide and 10g of ammonium polyvinyl alcohol phosphate, respectively dissolving in a small amount of solvent dissolving solution, mixing the three solutions together, shaking vigorously, mixing well, and diluting to 1000mL with a solvent.
3. The method for producing a novel methylene blue spectrophotometric absorbing solution as set forth in claim 2, wherein the solvent is water.
4. The method for preparing a novel methylene blue spectrophotometric absorbing solution as claimed in claim 1, wherein the step S1 comprises weighing 4.3g of cadmium sulfate, 0.3g of sodium hydroxide and 10g of arabinogalactan, respectively dissolving in a small amount of solvent, mixing the three solutions together, shaking vigorously, mixing well, and diluting to 1000mL with solvent.
5. The method for preparing a novel methylene blue spectrophotometric absorbing solution as claimed in claim 4, wherein the dissolving solution is water.
6. A novel methylene blue spectrophotometric absorbing solution, which is prepared by the preparation method of the novel methylene blue spectrophotometric absorbing solution as claimed in any one of claims 1 to 5.
7. A method for measuring hydrogen sulfide in a sewage treatment plant by using a novel methylene blue spectrophotometry absorbing solution prepared by the method for preparing a novel methylene blue spectrophotometry absorbing solution according to any one of claims 1 to 5, comprising the steps of:
step A, fully contacting the novel methylene blue spectrophotometry absorption liquid with waste gas of a sewage treatment station;
b, absorbing hydrogen sulfide in the waste gas by a novel methylene blue spectrophotometry absorption liquid to generate cadmium sulfide colloidal precipitate;
and step C, the sulfide ions and the p-aminodimethylaniline solution neutralize the ferric trichloride solution to generate methylene blue, and the methylene isatis root is observed according to the color depth and is measured by a spectrophotometry.
8. The method for measuring hydrogen sulfide in a sewage treatment plant according to claim 7, wherein the methylene blue spectrophotometry detection limit is 0.07 μ g/10mL, and when the volume of the sampled exhaust gas is 60L, the minimum detection concentration is 0.001mg/m3。
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007292565A (en) * | 2006-04-24 | 2007-11-08 | Toyo Seikan Kaisha Ltd | New methylene blue analytical method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007292565A (en) * | 2006-04-24 | 2007-11-08 | Toyo Seikan Kaisha Ltd | New methylene blue analytical method |
Non-Patent Citations (5)
| Title |
|---|
| 刘保献;马琳: "亚甲基蓝分光光度法测定环境空气中硫化氢的研究", 第十次全国环境监测学术交流会, 31 December 2011 (2011-12-31) * |
| 王云;王海燕;王新滨;: "硫化氢在吸收液采样过程中的稳定性", 职业与健康, no. 16, 15 August 2007 (2007-08-15) * |
| 王成;赵庆;: "氮氧化物和硫化氢常规化学监测法的反应机理", 油气田环境保护, no. 04, 28 August 2013 (2013-08-28), pages 43 * |
| 郑淑瑾, 刘其中: "空气中硫化氢测定方法的研究Ⅰ硫化氢在吸收液采样过程中的稳定性研究", 中国卫生检验杂志, no. 05, 20 October 1998 (1998-10-20), pages 269 - 270 * |
| 陆小妹;: "两种硫化氢测定方法的比较", 石油化工安全环保技术, no. 03, 20 June 2007 (2007-06-20), pages 52 - 53 * |
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