CN114088694A - Method for rapidly determining content of hydrogen sulfide in wastewater - Google Patents
Method for rapidly determining content of hydrogen sulfide in wastewater Download PDFInfo
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- CN114088694A CN114088694A CN202111225736.5A CN202111225736A CN114088694A CN 114088694 A CN114088694 A CN 114088694A CN 202111225736 A CN202111225736 A CN 202111225736A CN 114088694 A CN114088694 A CN 114088694A
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- silica gel
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000002351 wastewater Substances 0.000 title claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000741 silica gel Substances 0.000 claims abstract description 74
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 74
- 229940046892 lead acetate Drugs 0.000 claims abstract description 24
- 239000011521 glass Substances 0.000 claims abstract description 21
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000004043 dyeing Methods 0.000 claims abstract description 12
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 6
- 229940056932 lead sulfide Drugs 0.000 claims abstract description 4
- 229910052981 lead sulfide Inorganic materials 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000012937 correction Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 3
- 229940012189 methyl orange Drugs 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000007974 sodium acetate buffer Substances 0.000 claims description 3
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 2
- 238000002791 soaking Methods 0.000 claims 2
- 238000003756 stirring Methods 0.000 claims 2
- 238000004448 titration Methods 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 2
- 238000001816 cooling Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000009776 industrial production Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 238000004065 wastewater treatment Methods 0.000 abstract description 4
- 238000010186 staining Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for rapidly determining hydrogen sulfide content in wastewater, which comprises the steps of filling silica gel for chromatography, which is soaked with lead acetate, into a glass reaction tube, reacting the hydrogen sulfide of a sample with the lead acetate to generate brownish black lead sulfide when a wastewater sample is placed in the glass reaction tube, so that a dyeing layer with a certain length is shown on a silica gel layer, and determining the hydrogen sulfide content in the wastewater according to the volume of the silica gel of the dyeing layer. The method overcomes the defects of long time consumption, more detection steps and more factors influencing data accuracy in the traditional detection process of the content of the hydrogen sulfide; the method meets the requirement of quickly detecting the content of the hydrogen sulfide to effectively regulate and control production in industrial production, ensures the wastewater treatment effect, and effectively ensures the requirements of environmental-friendly emission reaching standards and recycling of production wastewater.
Description
Technical Field
The invention relates to the technical field of inspection and analysis, in particular to a method for rapidly determining the content of hydrogen sulfide in wastewater.
Background
In the industrial production process, a large amount of industrial wastewater is generated, particularly in the industries of coking, petroleum and steel, the detection of the components of the wastewater is very important, and the wastewater can be purposefully purified only by accurately detecting the components. Water is a source of life, is a fundamental stone for human beings to multiply and is the most precious resource in the nature. Water is the blood vessel of industrial production, and industrial production is difficult without water. Water, the origin of life, the source of civilization, the basis of ecology. China is a serious water-deficient country in the world, the per-capita water resource occupies 28% of the average level of the world, the water shortage in the country in normal years reaches 500 to billions of cubic meters, the water shortage is close to 2/3, the groundwater overstrain area in the country reaches 30 kilo-square kilometers.
Hydrogen sulfide in the wastewater is an important harmful component, the content of the hydrogen sulfide needs to be determined, particularly in industrial production, the content of the hydrogen sulfide needs to be rapidly detected so as to effectively regulate and control production, the traditional detection of the content of the hydrogen sulfide is performed by an iodometry method, but the method has the defects of long time consumption in the detection process, more detection steps, more factors influencing data accuracy, and difficulty in meeting the field production requirement in some cases, a method capable of rapidly detecting the content of the hydrogen sulfide needs to be determined, so that the production requirement of timely regulating and controlling production according to data is met, the wastewater treatment effect is guaranteed, and the requirements of environmental protection, standard discharge and recycling of production wastewater are guaranteed.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for rapidly determining the content of hydrogen sulfide in wastewater.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to a method for rapidly determining the content of hydrogen sulfide in wastewater, which comprises the steps of filling silica gel for chromatography, which is soaked with lead acetate, into a glass reaction tube, reacting the hydrogen sulfide of a sample with the lead acetate to generate brownish black lead sulfide when a wastewater sample is placed in the glass reaction tube, so that a dyeing layer with a certain length is displayed on a silica gel layer, and determining the content of the hydrogen sulfide in the wastewater according to the volume of the silica gel of the dyeing layer.
Further, the method comprises the following specific steps:
the first step is as follows: preparation and calibration of impregnated lead acetate silica gel
Weighing 20g of crystalline lead acetate, putting the crystalline lead acetate into a volumetric flask, adding 50mL of glacial acetic acid, adding 500mL of distilled water, shaking to dissolve the lead acetate, adding water to a scale mark, and shaking uniformly for later use; accurately measuring 20mL of the solution, putting the solution into a 250mL triangular flask, adding one drop of methyl orange indicator, adding ammonia water in a ratio of 1:1 to neutralize the solution, adding 20mL of acetic acid-sodium acetate buffer solution, 50mL of distilled water and one drop of xylenol orange indicator after the orange color is just yellow, titrating the solution by using an ethylene diamine tetraacetic acid disodium standard solution until the solution is at the end point from wine red to bright yellow, and performing a blank test when the solution is calibrated;
mg of lead per gram of impregnated silica gel:
in the formula: t is2-milligrams of lead per gram of impregnated silica gel;
T1-milligrams of lead per milliliter of solution in the preparation solution;
W1—the total weight of the impregnated silica gel;
then, filling the impregnated silica gel into the reaction tube, tightly knocking the impregnated silica gel to a scale, pouring the silica gel out of the reaction tube, and weighing the silica gel on an analytical balance;
mg lead per ml impregnated silica gel:
in the formula: t3-milligrams of lead per milliliter of impregnated silica gel;
T2-milligrams of lead per gram of impregnated silica gel;
W2- -weight of silica gel charged into the reaction tube used, g;
2- -represents the volume of the reaction tube, mL;
the impregnated silica gel per ml corresponds to micrograms of hydrogen sulfide:
in the formula: t isH2S-micrograms of hydrogen sulphide per ml of impregnated silica gel;
t3-milligrams of lead per milliliter of impregnated silica gel;
34- -molecular weight of hydrogen sulfide;
the third step: sealing one end of a dry and clean glass reaction tube with gauze, pouring silica gel impregnated with lead acetate from the other end, tamping and vertically placing on a reaction frame;
the fourth step: according to the property and condition of the waste water sample, the sample is pretreated, mainly comprising purification, decoloration and the like, so that the detection error of the sample caused by the self color is prevented and treated;
the fifth step: accurately transferring 0.2mL of the pretreated wastewater sample by using an injector, injecting the sample into a glass reaction tube, slightly pushing the glass injector to prevent the sample and silica gel from splashing out during injection, standing for 15 minutes, accurately reading the length of a silica gel dyeing layer after the sample completely and sufficiently reacts in the glass reaction tube, and calculating the content of hydrogen sulfide according to the volume of the dyeing layer;
and a sixth step: the content of the hydrogen sulfide is determined by the product of the volume of the dyed silica gel and the correction coefficient by adopting a correction coefficient method of a contrast experiment of a classical chemical method and a chromatography method.
Compared with the prior art, the invention has the beneficial technical effects that:
the method overcomes the defects that the traditional detection process of the content of the hydrogen sulfide is long in time consumption, multiple in detection steps and multiple in factors influencing data accuracy, and provides the method capable of rapidly detecting the content of the hydrogen sulfide. The method meets the requirement of quickly detecting the content of the hydrogen sulfide to effectively regulate and control production in industrial production, ensures the wastewater treatment effect, and effectively ensures the requirements of environmental-friendly emission reaching standards and recycling of production wastewater.
Detailed Description
A method for quickly measuring the content of hydrogen sulfide in waste water features that the silica gel impregnated with lead acetate for chromatography is put in a glass reaction tube, when the waste water sample is put in it, the hydrogen sulfide of the sample reacts with lead acetate to generate brownish black lead sulfide, resulting in a dyeing layer with a certain length on the silica gel layer, and the content of hydrogen sulfide in waste water is determined according to the volume of silica gel in the dyeing layer.
The method specifically comprises the following steps of,
firstly, preparing and calibrating lead acetate-impregnated silica gel, weighing 20g of crystalline lead acetate, putting the crystalline lead acetate into a volumetric flask, adding 50mL of glacial acetic acid, 500mL of distilled water, shaking to dissolve the lead acetate, adding water to a scale mark, and shaking uniformly for later use. Accurately measuring 20mL of the solution, putting the solution into a 250mL triangular flask, adding one drop of methyl orange indicator, adding ammonia water with the ratio of 1:1 to neutralize the solution, adding 20mL of acetic acid-sodium acetate buffer solution, 50mL of distilled water and one drop of xylenol orange indicator when the orange color is just yellow, titrating the solution by using an ethylene diamine tetraacetic acid disodium standard solution until the solution is from wine red to bright yellow, and performing a blank test when the solution is calibrated.
Mg of lead per gram of impregnated silica gel:
in the formula: t is2-milligrams of lead per gram of impregnated silica gel;
T1-milligrams of lead per milliliter of solution in the preparation solution;
W1—the total weight of the impregnated silica gel;
then, filling the impregnated silica gel into the reaction tube, tightly knocking the impregnated silica gel to a scale, pouring the silica gel out of the reaction tube, and weighing the silica gel on an analytical balance;
mg lead per ml impregnated silica gel:
in the formula: t3-milligrams of lead per milliliter of impregnated silica gel;
T2-milligrams of lead per gram of impregnated silica gel;
W2- -weight of silica gel charged into the reaction tube used, g;
2- -represents the volume of the reaction tube, mL;
the impregnated silica gel per ml corresponds to micrograms of hydrogen sulfide:
in the formula: t isH2S-micrograms of hydrogen sulphide per ml of impregnated silica gel;
t3-milligrams of lead per milliliter of impregnated silica gel;
34- -molecular weight of hydrogen sulfide;
and thirdly, taking a dry and clean glass reaction tube, sealing one end of the glass reaction tube by using gauze, pouring silica gel impregnated with lead acetate from the other end of the glass reaction tube, tamping and vertically placing the silica gel on a reaction frame.
And fourthly, according to the property and the condition of the wastewater sample, preprocessing the sample, mainly comprising purification, decoloration and the like, and preventing and treating the detection error of the sample caused by the self color.
And fifthly, accurately taking 0.2mL of the pretreated wastewater sample by using an injector, injecting the wastewater sample into a glass reaction tube, slightly pushing the glass injector to prevent the sample and the silica gel from splashing during injection, standing for 15 minutes, accurately reading the length of the silica gel staining layer after the sample completely and sufficiently reacts in the glass reaction tube, and calculating the content of the hydrogen sulfide according to the volume of the staining layer.
And sixthly, determining the content of the hydrogen sulfide by adopting a correction coefficient method of a contrast experiment of a classical chemical method and a chromatography method and according to the product of the volume of the dyed silica gel and the correction coefficient. The correction coefficient is strictly corrected periodically according to the change of seasonal temperature.
The invention overcomes the defects of long time consumption, more detection steps and more factors influencing data accuracy in the traditional detection process of the content of hydrogen sulfide, and provides a method capable of relatively quickly detecting the content of hydrogen sulfide. The method meets the requirement of quickly detecting the content of the hydrogen sulfide to effectively regulate and control production in industrial production, ensures the wastewater treatment effect, and effectively ensures the requirements of environmental-friendly emission reaching standards and recycling of production wastewater.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (2)
1. A method for rapidly determining the content of hydrogen sulfide in wastewater is characterized by comprising the following steps: the method comprises the steps of filling silica gel for chromatography, which is impregnated with lead acetate, into a glass reaction tube, reacting hydrogen sulfide of a sample with the lead acetate to generate brownish black lead sulfide when a wastewater sample is placed in the glass reaction tube, so that a dyeing layer with a certain length is displayed on a silica gel layer, and determining the content of the hydrogen sulfide in the wastewater according to the volume of the silica gel of the dyeing layer.
2. The method for rapidly determining the content of hydrogen sulfide in wastewater according to claim 1, which is characterized in that: the method comprises the following specific steps:
the first step is as follows: preparation and calibration of impregnated lead acetate silica gel
Weighing 20g of crystalline lead acetate, putting the crystalline lead acetate into a volumetric flask, adding 50mL of glacial acetic acid, adding 500mL of distilled water, shaking to dissolve the lead acetate, adding water to a scale mark, and shaking uniformly for later use; accurately measuring 20mL of the solution, putting the solution into a 250mL triangular flask, adding one drop of methyl orange indicator, adding ammonia water in a ratio of 1:1 to neutralize the solution, adding 20mL of acetic acid-sodium acetate buffer solution, 50mL of distilled water and one drop of xylenol orange indicator after the orange color is just yellow, titrating the solution by using an ethylene diamine tetraacetic acid disodium standard solution until the solution is at the end point from wine red to bright yellow, and performing a blank test when the solution is calibrated;
mg of lead per ml solution:
in the formula: a- -volume of standard solution consumed by titration of lead acetate solution, mL
A0Titration of the volume of standard solution consumed in the blank, mL
Molar concentration of M-disodium edetate standard solution
207- -molecular weight of lead
The second step is that: the preparation of the impregnated silica gel is carried out,
soaking silica gel in concentrated hydrochloric acid for 2 hours, washing with water, washing with distilled water to neutrality, drying at 120 ℃, taking 100g of dried silica gel, putting into a 500mL beaker, accurately weighing 20mL of lead acetate solution, mixing with 150mL of distilled water, pouring into the silica gel, fully stirring and soaking for 2 hours, then putting into a 65 +/-5 ℃ oven, stirring once every 30 minutes until the water content is 25-35%, taking out, cooling and weighing;
mg of lead per gram of impregnated silica gel:
in the formula: t is2-milligrams of lead per gram of impregnated silica gel;
T1-milligrams of lead per milliliter of solution in the preparation solution;
W1-total weight of impregnated silica gel;
then, filling the impregnated silica gel into the reaction tube, tightly knocking the impregnated silica gel to a scale, pouring the silica gel out of the reaction tube, and weighing the silica gel on an analytical balance;
mg lead per ml impregnated silica gel:
in the formula: t3-milligrams of lead per milliliter of impregnated silica gel;
T2-milligrams of lead per gram of impregnated silica gel;
W2- -weight of silica gel charged into the reaction tube used, g;
2- -represents the volume of the reaction tube, mL;
the impregnated silica gel per ml corresponds to micrograms of hydrogen sulfide:
in the formula: t isH2S-micrograms of hydrogen sulphide per ml of impregnated silica gel;
t3-milligrams of lead per milliliter of impregnated silica gel;
34- -molecular weight of hydrogen sulfide;
the third step: sealing one end of a dry and clean glass reaction tube with gauze, pouring silica gel impregnated with lead acetate from the other end, tamping and vertically placing on a reaction frame;
the fourth step: according to the property and condition of the waste water sample, the sample is pretreated, mainly comprising purification, decoloration and the like, so that the detection error of the sample caused by the self color is prevented and treated;
the fifth step: accurately transferring 0.2mL of the pretreated wastewater sample by using an injector, injecting the sample into a glass reaction tube, slightly pushing the glass injector to prevent the sample and silica gel from splashing out during injection, standing for 15 minutes, accurately reading the length of a silica gel dyeing layer after the sample completely and sufficiently reacts in the glass reaction tube, and calculating the content of hydrogen sulfide according to the volume of the dyeing layer;
and a sixth step: the content of the hydrogen sulfide is determined by the product of the volume of the dyed silica gel and the correction coefficient by adopting a correction coefficient method of a contrast experiment of a classical chemical method and a chromatography method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111225736.5A CN114088694A (en) | 2021-10-21 | 2021-10-21 | Method for rapidly determining content of hydrogen sulfide in wastewater |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111225736.5A CN114088694A (en) | 2021-10-21 | 2021-10-21 | Method for rapidly determining content of hydrogen sulfide in wastewater |
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