CN113237877A - Alkaline coal gangue alkalinity and heavy metal rapid release determination method - Google Patents
Alkaline coal gangue alkalinity and heavy metal rapid release determination method Download PDFInfo
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- CN113237877A CN113237877A CN202110523952.1A CN202110523952A CN113237877A CN 113237877 A CN113237877 A CN 113237877A CN 202110523952 A CN202110523952 A CN 202110523952A CN 113237877 A CN113237877 A CN 113237877A
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- coal gangue
- alkaline coal
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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
- G01N21/79—Photometric titration
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a method for measuring alkalinity and heavy metal release of alkaline coal gangue, which is characterized by comprising the following steps: (1) sample crushing treatment, and (2) measurement treatment. The method can effectively and rapidly measure the alkalinity and the leaching amount of heavy metal ions in the alkaline coal gangue in water environments with different pH values, and has the following advantages compared with the traditional static soaking method only setting the initial pH value condition: the data obtained by the experiment is that the alkalinity and the leaching amount of heavy metal ions of the alkaline coal gangue are measured when the alkaline coal gangue is placed in a water environment with a stable pH value, so that the natural condition is more appropriate; by adjusting the pH value of the alkaline coal gangue leachate, water environments with different pH values can be simulated; the way of releasing heavy metal ions is a static soaking way, and the maximum release amount of pollutants in the alkaline coal gangue can be reflected.
Description
Technical Field
The invention relates to the field of pollution control in mining areas, in particular to a method for rapidly releasing and measuring alkalinity and heavy metal of alkaline coal gangue.
Background
Coal gangue is a solid waste which is generated along with the coal mining and sorting process. At present, the total stacking amount of national coal gangue reaches 70 hundred million tons, the stacking amount is gradually increased at the speed of 1.5 to 2 hundred million tons per year, and the coal gangue is not only one of the most serious solid wastes stacked in a mining area, but also the industrial waste with the largest annual increment and storage amount and the largest land occupation in China. Along with the enhancement of environmental protection consciousness of people, the comprehensive utilization level of coal gangue in China is obviously improved, a large amount of coal gangue is applied to a plurality of fields such as filling and reclamation, sintering brick making, power generation, concrete material preparation and the like, and the coal industry development report in 2020 shows that the comprehensive utilization and disposal rate of the coal gangue in China reaches 72.2%, but a large amount of coal gangue is still stacked in the open air without being disposed. The coal gangue accumulated in the open air can occupy land resources, and can dissolve and release a large amount of toxic and harmful inorganic salt and heavy metal ions under the rainwater leaching effect, thereby causing serious harm to soil and underground water environment. Once people around a mining area contact or drink underground water with excessive heavy metal content, direct injury or indirect threat can be generated to human health, and different symptoms and influences are caused to the human body after excessive intake of different heavy metal elements, such as: iron (Fe) causes disorders of liver and spleen functions and skin pigmentation, manganese (Mn) causes people to show problems of neurasthenia, autonomic nervous dysfunction, etc., copper (Cu) causes damages of liver, kidney and nervous system, brain tissue lesion, zinc (Zn) causes damages of neurons and memory reduction, etc., chromium (Cr) causes damages to skin and respiratory tract, stimulates and corrodes mucous membrane.
At present, acidic coal gangue is mostly used as a research object for researching the release of pollutants in the coal gangue, the influence of different conditions on the change rule of each pollutant index in a leaching solution is researched through a soaking experiment, and the research on the alkalinity of alkaline coal gangue in water environments with different pH values and the release rule of heavy metal pollutants is relatively less at home and abroad. The invention can rapidly measure the alkalinity and the leaching amount of heavy metal elements in the alkaline coal gangue under water environments with different pH values, can be used for disclosing the release rule of the alkalinity and the heavy metal elements in the alkaline coal gangue, and provides experimental help for enriching the ecological management of mine environment and preventing and controlling the water environment pollution around the coal gangue hill.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for rapidly measuring the alkalinity and heavy metal release of alkaline coal gangue.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring alkalinity and heavy metal quick release of alkaline coal gangue comprises the following steps:
(1) and (3) sample crushing treatment:
taking an alkaline coal gangue sample to be measured by adopting a condensation method, placing the alkaline coal gangue sample in a constant-temperature air-blast drying box, drying the alkaline coal gangue sample to constant weight, and crushing the dried alkaline coal gangue sample by using a ball mill for later use;
(2) and (3) measurement treatment:
adding the alkaline coal gangue sample treated in the step (1) and deionized water into a beaker together, then placing the beaker on a magnetic stirrer for continuous stirring treatment, then carrying out acid titration treatment on the alkaline coal gangue leachate in the beaker by using an acid burette, repeatedly titrating to a preset pH value point, finishing titration when the alkaline coal gangue leachate does not change after the alkaline coal gangue leachate in the beaker reaches the preset point for 24 hours at the last time, and recording the accumulated acid consumption, namely converting the release amount of the alkalinity of the alkaline coal gangue; and then taking supernatant from the alkaline coal gangue leachate with the same pH value point, filtering by using a microporous filter membrane, taking 15ml of supernatant, putting the supernatant into a 50ml colorimetric tube, fully mixing, and measuring the concentration of heavy metal ions in the alkaline coal gangue leachate by using a flame atomic spectrophotometer.
Further, the temperature in the drying oven is controlled to 60 ℃ during the drying treatment in the step (1).
Further, the particle size of the crushed particles of the sample in the step (1) is less than 1 mm.
Further, the pore diameter of the microporous filter membrane in the step (2) is 0.45 μm.
The invention provides a method for rapidly measuring alkalinity and heavy metal release of alkaline coal gangue. Titrating the alkaline coal gangue leachate under static soaking to a preset pH value point by an acid titration method, determining the alkalinity release amount by acid consumption, simulating the pH value of the water environment where the coal gangue is located for a long time, filtering the alkaline coal gangue leachate with different pH values, and determining the mass concentration of heavy metal ions in the leachate.
Compared with the prior art, the invention has the beneficial effects that:
the method can effectively and rapidly measure the alkalinity and the leaching amount of heavy metal ions in the alkaline coal gangue in water environments with different pH values, and has the following advantages compared with the traditional static soaking method only setting the initial pH value condition: the data obtained by the experiment is that the alkalinity and the leaching amount of heavy metal ions of the alkaline coal gangue are measured when the alkaline coal gangue is placed in a water environment with a stable pH value, so that the natural condition is more appropriate; by adjusting the pH value of the alkaline coal gangue leachate, water environments with different pH values can be simulated; the way of releasing heavy metal ions is a static soaking way, and the maximum release amount of pollutants in the alkaline coal gangue can be reflected.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is a schematic diagram of the experimental method of example 1 of the present invention.
In the figure: 1. model ZJCG-3 magnetic stirrers; 2. PHS-3C type pH meter; 3. an acid burette; 4. and (4) a beaker.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Example 1
A method for measuring alkalinity and heavy metal quick release of alkaline coal gangue comprises the following steps:
(1) collecting alkaline coal gangue on site, taking a proper amount of alkaline coal gangue sample to be measured in a laboratory by adopting a condensation method, placing the alkaline coal gangue sample in a constant temperature blast drying oven, drying the alkaline coal gangue sample to constant weight at the temperature of 60 ℃, and crushing the dried coal gangue sample by using a ball mill until the particle size is less than 1 mm;
(2) weighing 20g of coal gangue powder sample by adopting an experimental device shown in figure 1, placing the coal gangue powder sample into a 250ml beaker 4, adding 200ml of deionized water, placing the beaker 4 on a ZJCG-3 type magnetic stirrer 1 for uninterrupted stirring, setting the rotating speed to be 800r/min, and fixing a PHS-3C type pH meter 2 into a sample leaching solution after stirring for 30min to monitor the change of the pH value in real time;
and recording the initial pH value of the coal gangue leachate, and replacing the rotor every 8 hours in order to prevent the influence on the test result caused by the reaction between the internal metal and the leachate after the surface coating of the magnetic rotor is damaged. Adding 1mol/L HNO into the beaker 4 by using an acid burette 3 for a plurality of times in a small amount during the stirring process3And (3) stabilizing the pH value of the solution to a preset value, titrating the pH value to the preset value, and keeping the leachate unchanged after 24 hours, namely, considering that the leachate reaches a preset point, and recording the acid consumption. In order to ensure the accuracy of experimental data, 3 groups of parallel experiments are carried out at the same preset pH value;
filtering supernatant of each group of leachate with the same pH value point with 0.45-micrometer microporous filter membrane, placing 15ml of each group of leachate into a 50ml colorimetric tube, fully mixing, and then measuring the concentration of heavy metal ions in the leachate with a flame atomic absorption spectrophotometer.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A method for measuring alkalinity and heavy metal quick release of alkaline coal gangue is characterized by comprising the following steps:
(1) and (3) sample crushing treatment:
taking an alkaline coal gangue sample to be measured by adopting a condensation method, placing the alkaline coal gangue sample in a constant-temperature air-blast drying box, drying the alkaline coal gangue sample to constant weight, and crushing the dried alkaline coal gangue sample by using a ball mill for later use;
(2) and (3) measurement treatment:
adding the alkaline coal gangue sample treated in the step (1) and deionized water into a beaker together, then placing the beaker on a magnetic stirrer for continuous stirring treatment, then carrying out acid titration treatment on the alkaline coal gangue leachate in the beaker by using an acid burette, repeatedly titrating to a preset pH value point, finishing titration when the alkaline coal gangue leachate does not change after the alkaline coal gangue leachate in the beaker reaches the preset point for 24 hours at the last time, and recording the accumulated acid consumption, namely converting the release amount of the alkalinity of the alkaline coal gangue; and then taking supernatant from the alkaline coal gangue leachate with the same pH value point, filtering by using a microporous filter membrane, taking 15ml of supernatant, putting the supernatant into a 50ml colorimetric tube, fully mixing, and measuring the concentration of heavy metal ions in the alkaline coal gangue leachate by using a flame atomic spectrophotometer.
2. The method for determining alkalinity and heavy metal release of alkaline coal gangue according to claim 1, wherein the temperature in the drying oven is controlled to be 60 ℃ during the drying treatment in step (1).
3. The method for measuring alkalinity and heavy metal release of alkaline coal gangue according to claim 1, wherein the particle size of the crushed sample in step (1) is less than 1 mm.
4. The method for determining alkalinity and heavy metal release of alkaline coal gangue according to claim 1, wherein the pore size of the microporous filter membrane in step (2) is 0.45 μm.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107727561A (en) * | 2017-10-11 | 2018-02-23 | 合肥学院 | A kind of agriculture and industry waste suppresses the test method of alum ore deposit hillock acidifying |
CN112285096A (en) * | 2020-09-28 | 2021-01-29 | 广东省科学院生态环境与土壤研究所 | Heavy metal contaminated soil ecological risk assessment method |
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- 2021-05-13 CN CN202110523952.1A patent/CN113237877A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107727561A (en) * | 2017-10-11 | 2018-02-23 | 合肥学院 | A kind of agriculture and industry waste suppresses the test method of alum ore deposit hillock acidifying |
CN112285096A (en) * | 2020-09-28 | 2021-01-29 | 广东省科学院生态环境与土壤研究所 | Heavy metal contaminated soil ecological risk assessment method |
Non-Patent Citations (5)
Title |
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PENG, BINGXIAN ET AL.: "Study on the release characteristics of chlorine in coal gangue under leaching conditions of different pH values", 《FUEL》 * |
曹云全等: "煤矸石中重金属动态淋滤和静态浸泡溶出特征研究", 《河北工程大学学报(自然科学版)》 * |
梁冰等: "不同pH值对磷矿废石磷素浸出特性影响的实验研究", 《地球与环境》 * |
王俭等: "浸提剂pH值对煤矸石和煤泥污染物浸出特性的影响研究", 《农业环境科学学报》 * |
王峰等: "定pH值下垃圾焚烧飞灰酸中和容量与元素浸出行为的研究", 《环境科学》 * |
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Application publication date: 20210810 |