CN114755352A - Method for measuring content of heavy metal elements in garbage and application - Google Patents
Method for measuring content of heavy metal elements in garbage and application Download PDFInfo
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- CN114755352A CN114755352A CN202210307266.5A CN202210307266A CN114755352A CN 114755352 A CN114755352 A CN 114755352A CN 202210307266 A CN202210307266 A CN 202210307266A CN 114755352 A CN114755352 A CN 114755352A
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 38
- 239000002893 slag Substances 0.000 claims abstract description 32
- 238000001514 detection method Methods 0.000 claims abstract description 25
- 239000012488 sample solution Substances 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 18
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims abstract description 17
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims abstract description 15
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 15
- 239000000287 crude extract Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 230000029087 digestion Effects 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 230000003009 desulfurizing effect Effects 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 160
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 87
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 75
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 58
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 51
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 49
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 37
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 30
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 25
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 25
- -1 hydroxide ions Chemical class 0.000 claims description 19
- 238000000120 microwave digestion Methods 0.000 claims description 17
- 239000000523 sample Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 13
- 239000002033 PVDF binder Substances 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 11
- 238000001195 ultra high performance liquid chromatography Methods 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 238000007865 diluting Methods 0.000 claims description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 7
- 238000001471 micro-filtration Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000012490 blank solution Substances 0.000 claims description 5
- 238000010828 elution Methods 0.000 claims description 5
- 238000010812 external standard method Methods 0.000 claims description 5
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical group O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012982 microporous membrane Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims 2
- 238000011084 recovery Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 14
- 239000002245 particle Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 238000005303 weighing Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for measuring the content of heavy metal elements in garbage and application thereof, wherein the method for measuring the content of the heavy metal elements in the garbage comprises the following steps: (1) grinding and crushing the slag blocks, adding a potassium carbonate solution for washing and desulfurizing, then filtering, and adding an alkali solution for digestion to obtain an alkaline hydrolysis sample solution; (2) adding a first acid solution into the alkaline hydrolysis sample solution in the step (1), adjusting the pH value to acidity, performing ultrasonic extraction, filtering, washing residues with a second acid solution, performing centrifugal separation, and extracting supernatant to obtain a crude extract; (3) and (3) concentrating the crude extract in the step (2), and filtering the concentrated solution to prepare a fine filtrate. The method for measuring the content of the heavy metal elements in the garbage has the advantages of high detection efficiency, high recovery rate, high precision, high treatment speed, simplicity and convenience in operation, wide application range and the like, and can be used for measuring various heavy metal elements.
Description
Technical Field
The invention belongs to the technical field of heavy metal detection, and particularly relates to a method for determining the content of heavy metal elements in garbage and application thereof.
Background
Heavy metals are pollutants existing in the environment for a long time and are a serious class influencing the quality of sediments due to the toxicity and the persistence of the heavy metals, and the heavy metals refer to the heavy metals with the atomic density of more than 5g/cm3About 45 kinds of metal elements ofSuch as copper, lead, zinc, cobalt, manganese, iron, cobalt, nickel, vanadium, zirconium, mercury, tungsten, aluminum, gold, silver, and the like. Although heavy metals such as manganese, copper and zinc are trace elements required for life activities, most of the heavy metals such as lead, fortune, mercury and the like are not required for life activities, and all the heavy metals are toxic to human bodies beyond a certain concentration. With the expansion of cities and the development of large-scale industry, heavy metal pollution in the atmosphere, soil and water environment is increasing. Heavy metal pollution is one of the main problems of water pollution, and artificial pollution such as mining, metal smelting, chemical production wastewater, pesticide and chemical fertilizer application, household garbage and the like, so that monitoring and control of heavy metal content become important problems related to environmental protection, sustainable development and improvement of resident living standard, and the conventional determination of heavy metal elements needs to carry out sample pretreatment on each heavy metal element independently, so that the workload is large, and the heavy metal detection efficiency is influenced.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for determining the content of heavy metal elements in garbage, wherein potassium carbonate solution is used to desulfurize slag, can avoid strong oxidation of hypochlorite ion to sulfur even under alkaline condition, so as to improve the accuracy of the experiment, the sample is pretreated by adopting an alkaline hydrolysis and acid extraction method subsequently, the loss of heavy metal elements and air pollution are avoided, the concentration step is added, the sensitivity of sample determination can be improved, meanwhile, the sample can be used for measuring various heavy metal elements after being pretreated, the pretreatment of each heavy metal element is not needed, the workload is reduced, the method is used for detecting the heavy metal elements in the garbage, the sensitivity is high, and has the advantages of high detection efficiency, good recovery rate, high precision, high processing speed, simple and convenient operation, wide application range and the like.
The invention also aims to provide the application of the method for determining the content of the heavy metal elements in the garbage.
In order to achieve the above object, an embodiment of the first aspect of the present invention provides a method for determining the content of heavy metal elements in garbage, including the following steps:
(1) Grinding and crushing the slag blocks, adding a potassium carbonate solution for washing and desulfurizing, then filtering, and adding an alkali solution for digestion to obtain an alkaline hydrolysis sample solution;
(2) adding a first acid solution into the alkaline hydrolysis sample solution in the step (1), adjusting the pH value to acidity, performing ultrasonic extraction, filtering, washing residues with a second acid solution, performing centrifugal separation, and extracting supernatant to obtain a crude extract;
(3) concentrating the crude extract in the step (2), and filtering the concentrated solution to prepare a fine filtrate;
(4) diluting the refined filtrate with a third acid solution and fixing the volume to obtain a test solution;
(5) preparing a blank solution according to the methods in the steps (1) to (4), and carrying out quantitative determination on the sample solution in the step (4) by adopting an ultra-high performance liquid chromatography;
the first acid solution, the second acid solution and the third acid solution are all acid solutions containing hypochlorous acid.
According to the method for determining the content of the heavy metal elements in the garbage, provided by the embodiment of the invention, the potassium carbonate solution is adopted to desulfurize the slag, so that hypochlorite can be prevented from having strong oxidizability even under an alkaline condition, sulfide ions can be oxidized into sulfur, the accuracy of an experiment is improved, an alkaline hydrolysis-acid extraction method is adopted to carry out pretreatment on a sample subsequently, the loss of the heavy metal elements and air pollution are avoided, a concentration step is added, the sensitivity of sample determination can be improved, the sample can be used for determining various heavy metal elements after pretreatment, each heavy metal element is not required to be subjected to independent pretreatment on the sample, the workload is reduced, and the method is used for detecting the heavy metal elements in the garbage, has the advantages of high sensitivity, high detection efficiency, good recovery rate, high processing speed, simplicity and convenience in operation, wide application range and the like.
In some embodiments of the invention, in step (1), the amount of the slag block is 6 to 10g, the amount of the potassium carbonate solution is 15 to 20mL, and the amount of the alkali solution is 8 to 12 mL; in the step (2), the dosage of the first acid solution is 20-24mL, and the dosage of the second acid solution is 10-12 mL; in the step (3), the fine filtrate is diluted by acid solution and the volume is 100 mL. In the method for measuring the content of heavy metal elements in garbage according to the embodiment of the present invention, the amount of each raw material reagent may be adjusted as needed, and is not limited to the above amount.
In some embodiments of the present invention, in step (1), the grinding can be performed in a mortar, or a grinding apparatus, such as a grinder. The particle size of the ground and crushed coal is 120-200 μm.
In some embodiments of the invention, in the step (1), the potassium carbonate content in the potassium carbonate solution is 30-50 wt%, the filtration is performed by using a microporous filtration membrane, the alkali solution is an alkali solution containing ammonia water, and the digestion is performed in a microwave digestion instrument.
In some embodiments of the present invention, in step (1), the microfiltration membrane is made of PVDF, the pore size of the microfiltration membrane is 50-100 μm, and the reference working conditions of the microwave digestion apparatus are as follows: the power is 1600-1800W, the heating time is 6-8min, the temperature is 130-200 ℃, and the holding time is 20-30 min.
In some embodiments of the present invention, in the step (1), the alkali solution containing ammonia water is a mixture of sodium hydroxide solution, potassium hydroxide solution and ammonia water, the concentration of hydroxide ions is 0.4 to 0.8mol/L, and the mass fraction of ammonia in the ammonia water is 9 to 12%. It should be noted that, the sodium hydroxide solution and the potassium hydroxide solution can be mixed in any ratio, and the content of sodium hydroxide in the sodium hydroxide solution and the content of potassium hydroxide in the potassium hydroxide solution are not limited, as long as the concentration of hydroxide ions is ensured to be between 0.4 mol/L and 0.8 mol/L.
In some embodiments of the present invention, in step (2), the pH adjusting agent is nitric acid, the pH is adjusted to 2-5, and ultrasonic extraction is performed by using an ultrasonic shaking device.
In some embodiments of the invention, in step (2), the power of ultrasonic extraction is 0.3-0.5KW, the frequency of ultrasonic extraction is 40-50kHz, the temperature of ultrasonic extraction is 35-55 ℃, and the time of ultrasonic extraction is 30-40 min. Preferably, the ultrasonic shaking device can be an ultrasonic extractor or the like.
According to the method for determining the content of the heavy metal elements in the garbage, disclosed by the embodiment of the invention, through setting the microwave digestion instrument and the ultrasonic shaking equipment for quick pretreatment, the sediment can be quickly digested, the digestion efficiency is improved, the working efficiency can be improved, and the input cost is reduced.
In some embodiments of the present invention, the acid solution containing hypochlorous acid is a mixture of a sulfuric acid solution, a hydrochloric acid solution, a citric acid solution, and a hypochlorous acid solution, a concentration of hydrogen ions is 0.2 to 0.5mol/L, and a mass fraction of hypochlorous acid in the hypochlorous acid solution is 4.5 to 5%. It should be noted that the sulfuric acid solution, the hydrochloric acid solution, and the citric acid solution may be mixed in any ratio, and the sulfuric acid content in the sulfuric acid solution, the hydrogen chloride content in the hydrochloric acid solution, and the citric acid content in the citric acid solution are not limited as long as the concentration of hydrogen ions is greater than or equal to 0.2-0.5 mol/L.
In some embodiments of the present invention, in step (3), the crude extract in step (2) is concentrated by using a distillation apparatus, and the concentrated solution is filtered by using a microporous membrane; in the step (3), the microfiltration membrane is made of PVDF (polyvinylidene fluoride), and the aperture of the microfiltration membrane is 5-50 microns. It should be noted that the distillation apparatus can be a conventional distillation apparatus (including a heating and vaporizing portion, a condensing portion, a receiving portion, etc., and generally including a thermometer, a round-bottomed flask, an alcohol burner, a condenser, a bullhorn, a conical flask, etc.) which is self-assembled in a laboratory, or a commercially available distillation apparatus, such as an intelligent distillation apparatus, etc.
In some embodiments of the present invention, in step (5), the ultra high performance liquid chromatography uses an ACQUITYUPLCBEHC18 column with a column size of 1.7 μm and 2.1 × 50mm, and the mobile phase is water-methanol gradient elution with a time of 0, 1.1, 2, 3, 4, 7, 8, 8.5, and 11 minutes, wherein the mass percentages of water and methanol are 100: 0,100: 0,98: 2,90: 10, 85: 15,0: 100,0: 100, 100: 0,100: 0, detection wavelength 254nm, flow rate 0.5 mL/min-1The amount of the sample was 5. mu.L, and the peak area was calculated by an external standard method.
In order to achieve the above purpose, an embodiment of the second aspect of the present invention provides an application of the method for determining the content of heavy metal elements in garbage in the field of garbage detection.
The application of the method for determining the content of the heavy metal elements in the garbage in the embodiment of the invention in the field of garbage detection is basically the same as the beneficial effects of the method for determining the content of the heavy metal elements in the garbage, and the method is not repeated herein.
Additional aspects and advantages of the present application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the present application.
Detailed Description
The following detailed description describes embodiments of the present application, which are exemplary and are intended to be illustrative of the present application and are not to be construed as limiting the present application.
The raw material reagents and equipment used in the examples and comparative examples of the present invention are commercially available reagents or equipment unless otherwise specified; the experimental methods used in the examples and comparative examples of the present invention are conventional experimental methods unless otherwise specified.
The distillation apparatuses referred to in the following examples and comparative examples of the present invention are all conventional distillation apparatuses (including a heat vaporization section, a condensation section, a receiving section, etc., generally including a thermometer, a round-bottomed flask, an alcohol lamp, a condenser tube, a bull horn, a conical flask, etc.) which are self-assembled in a laboratory.
First, examples and comparative examples
Example 1
A method for measuring the content of heavy metal elements in garbage comprises the following steps:
(1) weighing 8g of slag block, grinding and crushing the slag block by using a mortar until the particle size is 120-200 mu m, adding 15mL of potassium carbonate solution (the content of the potassium carbonate is 30.0 wt%) for washing and desulfurizing, filtering the slag block by using a 50-100 mu m microporous filter membrane made of PVDF material, placing the filtered slag block into a digestion tank of a microwave digestion instrument, and adding 9mL of aqueous alkali containing ammonia to obtain an alkaline hydrolysis sample solution. Wherein the aqueous alkali containing the ammonia water is a mixture of the ammonia water, a sodium hydroxide solution and a potassium hydroxide solution (the pH value of the ammonia water is adjusted to 13.78 after the sodium hydroxide solution and the potassium hydroxide solution are mixed according to the volume ratio of 1: 1, wherein the sodium hydroxide content in the sodium hydroxide solution is 50.0 wt%, the potassium hydroxide content in the potassium hydroxide solution is 45.0 wt%), the concentration of hydroxide ions is 0.4mol/L, and the mass fraction of ammonia in the ammonia water is 9%; the reference working conditions of the microwave digestion instrument are as follows: the power is 1600W, the heating time is 6min, the temperature is 130 ℃, and the holding time is 20 min.
(2) Adding 20mL of acid solution containing hypochlorous acid into the alkaline hydrolysis sample solution obtained in the step (1) rapidly (within 5-10 s) under the condition of magnetic stirring, detecting the pH value of the solution, adjusting the pH value to 2 by using nitric acid, performing ultrasonic extraction for 30min by using an ultrasonic extractor under the conditions of 37 ℃ and 0.3KW and 42kHz, performing centrifugal separation by using a centrifugal machine, washing the filtered residue by using 10mL of acid solution containing hypochlorous acid, performing centrifugal treatment by using the centrifugal machine, and extracting supernatant to obtain a crude extract. Wherein the acid solution containing hypochlorous acid is a hypochlorous acid solution, a sulfuric acid solution, a mixture of a hydrochloric acid solution and a citric acid solution (the pH of the hypochlorous acid solution is adjusted to 0.70 after the sulfuric acid solution, the hydrochloric acid solution and the citric acid solution are mixed according to the volume ratio of 1: 1: 1, wherein the sulfuric acid content in the sulfuric acid solution is 18 wt%, the hydrogen chloride content in the hydrochloric acid solution is 10 wt%, the citric acid content in the citric acid solution is 5 wt%), and the concentration of hydrogen ions is equal to 0.2 mol/L; the mass fraction of hypochlorous acid in the hypochlorous acid solution is 4.5%.
(3) Concentrating the crude extract in the step (2) by adopting a distillation device to prepare a concentrated solution; then filtering the concentrated solution with PVDF microporous membrane of 5-50 μm to obtain the fine filtrate.
(4) Diluting the fine filtrate with an acid solution containing hypochlorous acid, and diluting to 100mL to obtain a sample solution. Wherein the acid solution containing hypochlorous acid is a hypochlorous acid solution, a sulfuric acid solution, a mixture of a hydrochloric acid solution and a citric acid solution (the pH of the hypochlorous acid solution is adjusted to 0.70 after the sulfuric acid solution, the hydrochloric acid solution and the citric acid solution are mixed according to the volume ratio of 1: 1: 1, wherein the sulfuric acid content in the sulfuric acid solution is 15 wt%, the hydrogen chloride content in the hydrochloric acid solution is 7 wt%, the citric acid content in the citric acid solution is 3 wt%), and the concentration of hydrogen ions is equal to 0.2 mol/L; the mass fraction of hypochlorous acid in the hypochlorous acid solution is 4.5%.
(5) According to the steps (1) to (4), the slag block sample test solutionThe preparation method of (4) is characterized in that a blank solution is prepared, and then the sample solution in the step (4) is quantitatively measured by adopting ultra-high performance liquid chromatography. Wherein the chromatographic column used by the ultra-high performance liquid chromatography is ACQUITYUPLCBEHC18, the specification of the chromatographic column is 1.7 mu m and 2.1 x 50mm, the mobile phase is water-methanol gradient elution, the time is 0, 1.1, 2, 3, 4, 7, 8, 8.5, and the mass percentages of water and methanol are respectively 100 when the time is 11 minutes: 0,100: 0,98: 2,90: 10, 85: 15,0: 100,0: 100, 100: 0,100: 0, detection wavelength 254nm, flow rate 0.5 mL/min -1The amount of the sample was 5. mu.L, and the peak area was calculated by an external standard method.
Example 2
A method for measuring the content of heavy metal elements in garbage comprises the following steps:
(1) weighing 8g of slag block, grinding and crushing the slag block by using a grinder until the particle size is 120-200 mu m, adding 15mL of potassium carbonate solution (the content of the potassium carbonate is 50 wt%) to wash and remove sulfur, filtering the slag block by using a PVDF (polyvinylidene fluoride) microporous filter membrane with the particle size of 50-100 mu m, placing the filtered slag block into a digestion tank of a microwave digestion instrument, and adding 12mL of aqueous alkali containing ammonia to obtain an alkaline hydrolysis sample solution. Wherein the aqueous alkali containing the ammonia water is a mixture of the ammonia water, a sodium hydroxide solution and a potassium hydroxide solution (the pH value of the ammonia water is adjusted to 13.90 after the sodium hydroxide solution and the potassium hydroxide solution are mixed according to the volume ratio of 1: 1, wherein the sodium hydroxide content in the sodium hydroxide solution is 50.0 wt%, the potassium hydroxide content in the potassium hydroxide solution is 45.0 wt%), the concentration of hydroxide ions is 0.8mol/L, and the mass fraction of ammonia in the ammonia water is 12%; the reference working conditions of the microwave digestion instrument are as follows: the power is 1800W, the heating time is 8min, the temperature is 200 ℃, and the holding time is 30 min.
(2) Rapidly (within 5-10 s) adding 24mL of acid solution containing hypochlorous acid into the alkaline hydrolysis sample solution obtained in the step (1) under the condition of magnetic stirring, detecting the pH value of the solution, adjusting the pH value to 5 by using nitric acid, ultrasonically extracting for 40min by using an ultrasonic extractor under the conditions of 45 ℃, 0.5KW and 45kHz, then centrifugally separating by using a centrifuge, washing filtered residues by using 12mL of acid solution containing hypochlorous acid, centrifugally treating by using the centrifuge, and extracting supernatant to obtain a crude extract. Wherein the acid solution containing hypochlorous acid is a hypochlorous acid solution, a sulfuric acid solution, a mixture of a hydrochloric acid solution and a citric acid solution (the pH of the hypochlorous acid solution is adjusted to 0.30 after the sulfuric acid solution, the hydrochloric acid solution and the citric acid solution are mixed according to the volume ratio of 1: 1: 1, wherein the sulfuric acid content in the sulfuric acid solution is 35 wt%, the hydrogen chloride content in the hydrochloric acid solution is 20 wt%, the citric acid content in the citric acid solution is 10 wt%), and the concentration of hydrogen ions is 0.5 mol/L; the mass fraction of hypochlorous acid in the hypochlorous acid solution is 5 percent.
(3) Concentrating the crude extract in the step (2) by adopting a distillation device to prepare a concentrated solution; then filtering the concentrated solution with PVDF microporous membrane of 5-50 μm to obtain the fine filtrate.
(4) Diluting the fine filtrate with an acid solution containing hypochlorous acid, and diluting to 100mL to obtain a sample solution. Wherein the acid solution containing hypochlorous acid is a hypochlorous acid solution, a sulfuric acid solution, a mixture of a hydrochloric acid solution and a citric acid solution (the pH value of the hypochlorous acid solution is adjusted to 0.30 after the sulfuric acid solution, the hydrochloric acid solution and the citric acid solution are mixed according to the volume ratio of 1: 1: 1, wherein the sulfuric acid content in the sulfuric acid solution is 25 wt%, the hydrogen chloride content in the hydrochloric acid solution is 15 wt%, the citric acid content in the citric acid solution is 6 wt%), and the concentration of hydrogen ions is 0.5 mol/L; the mass fraction of hypochlorous acid in the hypochlorous acid solution is 5 percent.
(5) Preparing a blank solution according to the preparation method of the test sample solution of the slag block sample in the steps (1) to (4), and then carrying out quantitative determination on the test sample solution in the step (4) by adopting ultra-high performance liquid chromatography. Wherein a chromatographic column used by the ultra-high performance liquid chromatography is ACQUITYUPLCBEHC18, the specification of the chromatographic column is 1.7 mu m and 2.1 x 50mm, the mobile phase is water-methanol gradient elution, the time is 0, 1.1, 2, 3, 4, 7, 8 and 8.5 respectively, and the mass percentages of water and methanol are 100 respectively when 11 minutes occur: 0,100: 0,98: 2,90: 10, 85: 15,0: 100,0: 100, 100: 0,100: 0, detection wavelength 254nm, flow rate 0.5 mL/min -1The amount of the sample was 5. mu.L, and the peak area was calculated by an external standard method.
Example 3
A method for measuring the content of heavy metal elements in garbage comprises the following steps:
(1) weighing 8g of slag block, grinding and crushing the slag block by using a mortar until the particle size is 120-200 mu m, adding 15mL of potassium carbonate solution (the content of the potassium carbonate is 40 wt%) to wash and remove sulfur, filtering the slag block by using a PVDF (polyvinylidene fluoride) microporous filter membrane with the particle size of 50-100 mu m, placing the filtered slag block into a digestion tank of a microwave digestion instrument, and adding 11mL of aqueous alkali containing ammonia to obtain an alkaline hydrolysis sample solution. Wherein the aqueous alkali containing the ammonia water is a mixture of the ammonia water, a sodium hydroxide solution and a potassium hydroxide solution (the pH value of the ammonia water is adjusted to 13.78 after the sodium hydroxide solution and the potassium hydroxide solution are mixed according to the volume ratio of 1: 1, wherein the sodium hydroxide content in the sodium hydroxide solution is 50.0 wt%, the potassium hydroxide content in the potassium hydroxide solution is 45.0 wt%), the concentration of hydroxide ions is 0.6mol/L, and the mass fraction of ammonia in the ammonia water is 11%; the reference working conditions of the microwave digestion instrument are as follows: the power is 1700W, the heating time is 7min, the temperature is 165 ℃, and the holding time is 25 min.
(2) Adding 22mL of acid solution containing hypochlorous acid into the alkaline hydrolysis sample solution obtained in the step (1) rapidly (within 5-10 s) under the condition of magnetic stirring, detecting the pH value of the solution, adjusting the pH value to 4 by using nitric acid, performing ultrasonic extraction for 35min by using an ultrasonic extractor under the conditions of 45 ℃, 0.4KW and 48kHz, performing centrifugal separation by using a centrifugal machine, washing filtered residues by using 12mL of acid solution containing hypochlorous acid, performing centrifugal treatment by using the centrifugal machine, and extracting supernatant to obtain a crude extract. Wherein the acid solution containing hypochlorous acid is hypochlorous acid solution, sulfuric acid solution, a mixture of hydrochloric acid solution and citric acid solution (after the sulfuric acid solution, the hydrochloric acid solution and the citric acid solution are mixed according to the volume ratio of 1: 1: 1, the pH value of the hypochlorous acid solution is adjusted to 0.40, the sulfuric acid content in the sulfuric acid solution is 22 wt%, the hydrogen chloride content in the hydrochloric acid solution is 12 wt%, the citric acid content in the citric acid solution is 6 wt%), and the concentration of hydrogen ions is 0.4 mol/L; the mass fraction of hypochlorous acid in the hypochlorous acid solution is 4.8%.
(3) Concentrating the crude extract in the step (2) by adopting a distillation device to prepare a concentrated solution; then filtering the concentrated solution with PVDF microporous membrane of 5-50 μm to obtain fine filtrate.
(4) Diluting the fine filtrate with acid solution containing hypochlorous acid, and diluting to 100mL to obtain sample solution. Wherein the acid solution containing hypochlorous acid is a hypochlorous acid solution, a sulfuric acid solution, a mixture of a hydrochloric acid solution and a citric acid solution (the pH of the hypochlorous acid solution is adjusted to 0.40 after the sulfuric acid solution, the hydrochloric acid solution and the citric acid solution are mixed according to the volume ratio of 1: 1: 1, wherein the sulfuric acid content in the sulfuric acid solution is 16 wt%, the hydrogen chloride content in the hydrochloric acid solution is 8 wt%, the citric acid content in the citric acid solution is 4 wt%), and the concentration of hydrogen ions is 0.4 mol/L; the mass fraction of hypochlorous acid in the hypochlorous acid solution is 4.8%.
(5) Preparing a blank solution according to the preparation method of the slag block sample test solution in the steps (1) to (4), and then carrying out quantitative determination on the test solution in the step (4) by adopting an ultra-high performance liquid chromatography. Wherein the chromatographic column used by the ultra-high performance liquid chromatography is ACQUITYUPLCBEHC18, the specification of the chromatographic column is 1.7 mu m and 2.1 x 50mm, the mobile phase is water-methanol gradient elution, the time is 0, 1.1, 2, 3, 4, 7, 8, 8.5, and the mass percentages of water and methanol are respectively 100 when the time is 11 minutes: 0,100: 0,98: 2,90: 10, 85: 15,0: 100,0: 100, 100: 0,100: 0, detection wavelength 254nm, flow rate 0.5 mL/min -1The amount of the sample was 5. mu.L, and the peak area was calculated by an external standard method.
Comparative example 1
The method for measuring the content of the heavy metal elements in the garbage of the comparative example is basically the same as that of the example 2, except that: and (2) washing and desulfurizing without a potassium carbonate solution in the step (1), and directly placing the ground slag blocks in a microwave digestion instrument. Namely, the step (1) is as follows: weighing 8g of slag block, grinding and crushing the slag block by using a grinder until the particle size is 120-200 mu m, adding 15mL of potassium carbonate solution (the content of the potassium carbonate is 50 wt%) to wash and remove sulfur, filtering the slag block by using a PVDF (polyvinylidene fluoride) microporous filter membrane with the particle size of 50-100 mu m, placing the filtered slag block into a digestion tank of a microwave digestion instrument, and adding 12mL of aqueous alkali containing ammonia to obtain an alkaline hydrolysis sample solution. Wherein the aqueous alkali containing the ammonia water is a mixture of the ammonia water, a sodium hydroxide solution and a potassium hydroxide solution (the pH value of the ammonia water is adjusted to 13.90 after the sodium hydroxide solution and the potassium hydroxide solution are mixed according to the volume ratio of 1: 1, wherein the sodium hydroxide content in the sodium hydroxide solution is 50.0 wt%, the potassium hydroxide content in the potassium hydroxide solution is 45.0 wt%), the concentration of hydroxide ions is 0.8mol/L, and the mass fraction of ammonia in the ammonia water is 12%; the reference working conditions of the microwave digestion instrument are as follows: the power is 1800W, the heating time is 8min, the temperature is 200 ℃, and the holding time is 30 min.
Comparative example 2
The method for measuring the content of the heavy metal elements in the garbage of the comparative example is basically the same as that of the example 3, and the difference is that: and (2) washing and desulfurizing without potassium carbonate solution in the step (1), and directly putting the ground slag block into a microwave digestion instrument. Namely, the step (1) is as follows: weighing 8g of slag block, grinding and crushing the slag block by using a mortar until the particle size is 120-200 mu m, adding 15mL of potassium carbonate solution (the content of the potassium carbonate is 40 wt%) to wash and remove sulfur, filtering the slag block by using a PVDF (polyvinylidene fluoride) microporous filter membrane with the particle size of 50-100 mu m, placing the filtered slag block into a digestion tank of a microwave digestion instrument, and adding 11mL of aqueous alkali containing ammonia to obtain an alkaline hydrolysis sample solution. Wherein the aqueous alkali containing the ammonia water is a mixture of the ammonia water, a sodium hydroxide solution and a potassium hydroxide solution (the pH value of the ammonia water is adjusted to 13.78 after the sodium hydroxide solution and the potassium hydroxide solution are mixed according to the volume ratio of 1: 1, wherein the sodium hydroxide content in the sodium hydroxide solution is 50.0 wt%, the potassium hydroxide content in the potassium hydroxide solution is 45.0 wt%), the concentration of hydroxide ions is 0.6mol/L, and the mass fraction of ammonia in the ammonia water is 11%; the reference working conditions of the microwave digestion instrument are as follows: the power is 1700W, the heating time is 7min, the temperature is 165 ℃, and the holding time is 25 min.
Second, the detection result
The heavy metal content of the same garbage furnace slag blocks in a certain place is detected by adopting the detection methods of the examples 1-3 and the comparative examples 1 and 2 respectively (wherein the comparative example 1 and the comparative example 2 do not carry out washing desulphurization operation by potassium carbonate solution), and the detection results are shown in table 1.
TABLE 1 test results of the test methods of examples 1 to 3 and comparative example
As can be seen from table 1, compared with comparative example 1 and comparative example 2, the data obtained in example 1, example 2 and example 3 are closer to the reference values, and thus it is confirmed that the accuracy of the detection of the metal element can be improved by adding the potassium carbonate solution for washing and desulfurizing, which is necessary.
In the present disclosure, the terms "one embodiment," "some embodiments," "example," "specific example," or "some examples" and the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Moreover, various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art without being mutually inconsistent.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for measuring the content of heavy metal elements in garbage is characterized by comprising the following steps:
(1) grinding and crushing the slag blocks, adding a potassium carbonate solution for washing and desulfurizing, then filtering, and adding an alkali solution for digestion to obtain an alkaline hydrolysis sample solution;
(2) adding a first acid solution into the alkaline hydrolysis sample solution in the step (1), adjusting the pH value to acidity, performing ultrasonic extraction, filtering, washing residues with a second acid solution, performing centrifugal separation, and extracting supernatant to obtain a crude extract;
(3) concentrating the crude extract in the step (2), and filtering the concentrated solution to prepare a fine filtrate;
(4) diluting the refined filtrate with a third acid solution and fixing the volume to obtain a test solution;
(5) preparing a blank solution according to the methods in the steps (1) to (4), and quantitatively measuring the test sample solution in the step (4) by adopting ultra-high performance liquid chromatography;
The first acid solution, the second acid solution and the third acid solution are all acid solutions containing hypochlorous acid.
2. The detection method according to claim 1, wherein in the step (1), the potassium carbonate content in the potassium carbonate solution is 30-50 wt%, the filtration is performed by using a microfiltration membrane, the alkaline solution is an alkaline solution containing ammonia water, and the digestion is performed in a microwave digestion instrument.
3. The detection method according to claim 2, wherein in the step (1), the microfiltration membrane is made of PVDF, and the microwave digestion instrument has the reference working conditions: the power is 1600-1800W, the temperature rise time is 6-8min, the temperature is 130-200 ℃, and the holding time is 20-30 min.
4. The detection method according to claim 2, wherein in the step (1), the aqueous alkali containing ammonia is a mixture of a sodium hydroxide solution, a potassium hydroxide solution and ammonia, the concentration of hydroxide ions is 0.4 to 0.8mol/L, and the mass fraction of ammonia in the ammonia is 9 to 12%.
5. The detection method according to claim 1, wherein in the step (2), the pH regulator is nitric acid, the pH is adjusted to 2-5, and ultrasonic extraction is performed by using an ultrasonic shaking device.
6. The detection method according to claim 5, wherein in the step (2), the power of ultrasonic extraction is 0.3-0.5KW, the frequency of ultrasonic extraction is 40-50kHz, the temperature of ultrasonic extraction is 35-55 ℃, and the time of ultrasonic extraction is 30-40 min.
7. The detection method according to claim 1, wherein the acid solution containing hypochlorous acid is a mixture of a sulfuric acid solution, a hydrochloric acid solution, a citric acid solution, and a hypochlorous acid solution, the concentration of hydrogen ions is 0.2 to 0.5mol/L, and the mass fraction of hypochlorous acid in the hypochlorous acid solution is 4.5 to 5%.
8. The detection method according to claim 1, wherein in the step (3), the crude extract in the step (2) is concentrated by a distillation device, and the concentrated solution is filtered by a microporous membrane; in the step (3), the microporous filter membrane is made of PVDF.
9. The detection method according to claim 1, wherein in the step (5), the ultra high performance liquid chromatography is performed by using an ACQUITYUPLCBEHC18 as a chromatographic column, the specification of the chromatographic column is 1.7 μm, the size of the chromatographic column is 2.1X 50mm, and the mobile phase is water-methanol gradient elution with the time of 0, 1.1, 2, 3, 4, 7, 8, 8.5 and the mass percentages of water and methanol at 11 minutes are respectively 100: 0,100: 0,98: 2,90: 10, 85: 15,0: 100,0: 100, 100: 0,100: 0, detection wavelength 254nm, flow rate 0.5 mL/min-1The amount of the sample was 5. mu.L, and the peak area was calculated by an external standard method.
10. The application of the method for determining the content of the heavy metal elements in the garbage according to any one of claims 1 to 9 in the field of garbage detection.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784864A (en) * | 2016-03-10 | 2016-07-20 | 山东五洲检测有限公司 | Detection method of heavy metal in soil |
| CN108531736A (en) * | 2018-04-25 | 2018-09-14 | 华中科技大学 | A method of it is cleaned by scrap lead cream hydrometallurgic recovery and prepares high-purity lead compound |
| CN109959727A (en) * | 2017-12-26 | 2019-07-02 | 湖南泰华科技检测有限公司 | A kind of application of chemical reagent formulation in detection heavy metal pollution of soil |
| CN110607454A (en) * | 2019-09-29 | 2019-12-24 | 新中天环保股份有限公司 | Method for extracting heavy metal from secondary fly ash generated in waste incineration |
| KR102177160B1 (en) * | 2020-06-17 | 2020-11-10 | 주식회사 이지 | Composition for removing SOxandstabilizing heavy metals |
-
2022
- 2022-03-25 CN CN202210307266.5A patent/CN114755352A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784864A (en) * | 2016-03-10 | 2016-07-20 | 山东五洲检测有限公司 | Detection method of heavy metal in soil |
| CN109959727A (en) * | 2017-12-26 | 2019-07-02 | 湖南泰华科技检测有限公司 | A kind of application of chemical reagent formulation in detection heavy metal pollution of soil |
| CN108531736A (en) * | 2018-04-25 | 2018-09-14 | 华中科技大学 | A method of it is cleaned by scrap lead cream hydrometallurgic recovery and prepares high-purity lead compound |
| CN110607454A (en) * | 2019-09-29 | 2019-12-24 | 新中天环保股份有限公司 | Method for extracting heavy metal from secondary fly ash generated in waste incineration |
| KR102177160B1 (en) * | 2020-06-17 | 2020-11-10 | 주식회사 이지 | Composition for removing SOxandstabilizing heavy metals |
Non-Patent Citations (1)
| Title |
|---|
| 李连山 等: "《大气污染控制工程》", 31 August 2003, 武汉理工大学出版社, pages: 270 - 271 * |
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