CN104034720A - Detection method for heavy metal in building wastes - Google Patents
Detection method for heavy metal in building wastes Download PDFInfo
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- CN104034720A CN104034720A CN201410245673.3A CN201410245673A CN104034720A CN 104034720 A CN104034720 A CN 104034720A CN 201410245673 A CN201410245673 A CN 201410245673A CN 104034720 A CN104034720 A CN 104034720A
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Abstract
The invention relates to a detection method for heavy metal in building wastes. The detection method comprises the following steps: preparing 100g of the building wastes polluted by the heavy metal; carrying out pre-treatment and carrying out quartering division; randomly selecting one part and drying for one hour at 100 DEG C; crushing the dried building wastes in a sealed manner until the grain diameter is less than 180 microns; then weighing 0.1-0.3g of the building wastes and laying on watch glass; drying the watch glass in a drying oven at 100 DEG C for two hours until the weight is constant; placing the building waste powder into a polytetrafluoroethylene crucible; adding 9mL of nitrohydrochloric acid and immersing for 10 minutes; adding 1mL of 40% hydrofluoric acid; covering the crucible and heating the crucible on an electric heating plate of 180 DEG C until solids are dissolved; adding 30mL of de-ionized water into the polytetrafluoroethylene crucible and continuing heating and steaming until 2-5mL of liquid is left; and finally, after cooling the polytetrafluoroethylene crucible to a room temperature, transferring liquid in the crucible to a plastic volumetric flask; making up to volume of 100mL by using a 4% nitric acid solution; and determining the content of the heavy metal in the solution by adopting an ICP-OES (Inductively Coupled Plasma Optical Emission Spectroscopy). The detection is accurate and credible.
Description
Technical field
The present invention relates to heavy metal detection method in a kind of waste material of buildings.Belong to content of beary metal detection technique field in waste material of buildings.
Background technology
The quick propelling with urbanization process that develops rapidly along with China's economy, removal, reorganization and expansion and new project produce a large amount of waste material of buildings, producing every year according to estimates building waste is 2,400,000,000 tons of left and right, the contaminated waste material of buildings producing comprising removal or the reconstruction of a large amount of chemical industry, metallurgy, light industry, processing enterprise.Detect content of beary metal in waste material of buildings, differentiate common buildings refuse and contaminated waste material of buildings, investigate the pollution situation of waste material of buildings, be beneficial to the further harmless resource utilization of waste material of buildings.But waste material of buildings character is special, before detection, need to carry out certain pre-service.For example concrete, fragment of brick class waste material of buildings quality are hard, contain the materials such as a large amount of silicon dioxide, and the dust of crushing process is revealed and digestion process not exclusively all can cause last mensuration inaccurate.
Lack at present the standard method that waste material of buildings content of beary metal is measured both at home and abroad, the digestion procedures that adopt heavy metal in soil in literature research more, the method acid consumption is large, as heavy metal in waste material of buildings, clear up, its accuracy quantitatively judges, in a word, the accurate method that in so far there are no waste material of buildings, content of beary metal detects, also lacks the recovery of standard addition checking detecting about content of beary metal in waste material of buildings.
Summary of the invention
The object of this invention is to provide the method that heavy metal in a kind of waste material of buildings detects, specifically for detection of the disposal route of zinc, copper, lead, chromium content in waste material of buildings.
For reaching above-mentioned purpose, the present invention is directed in waste material of buildings content of beary metal and detect feature, first successively according to dry, broken, pulverize, clear up and carry out pre-service, then constant volume, measure and calculate content of beary metal in waste material of buildings.Concrete steps are as follows:
First get the contaminated by heavy metals waste material of buildings of 100g, carry out inquartation division after pre-service, choose at random a copy of it and at 100 ℃, dry 1 hour; The waste material of buildings sealing of drying is pulverized 1 minute, be less than 180 μ m to particle diameter; Then take 0.1g-0.3g and be laid on surface plate, be placed in that 100 ℃ of baking ovens are dry dries 2 hours to constant weight; Waste material of buildings powder is placed in teflon crucible again, adds chloroazotic acid 9mL, soak and add 1mL40% hydrofluorite after 10 minutes, crucible is added a cover to be placed on 180 ℃ of electric hot plates and is heated to dissolution of solid; Then in teflon crucible, add 30mL deionized water, continue hot digestion to 2-5mL; Finally, after teflon crucible cool to room temperature, liquid rotating in crucible is moved to plastics volumetric flask, with 4% salpeter solution, be settled to 100mL; Adopt ICP-OES to measure content of beary metal in solution, calculate content of beary metal in waste material of buildings;
After above-mentioned waste material of buildings sample pretreatment, the method for inquartation division is: 100 ℃, waste material of buildings sample is dried 24 hours; Adopt jaw crusher or manually block waste material of buildings sample carried out to preliminary fragmentation, the more block waste material of buildings of preliminary fragmentation is fully mixed, tiling, with inquartation division;
Above-mentioned contaminated by heavy metals waste material of buildings is by the waste material of buildings of the pollution of zinc, copper, lead, chromium.
Described chloroazotic acid, for now joining chloroazotic acid, measures hydrochloric acid: nitric acid=3:1 volume ratio, mixes.Hydrochloric acid used and nitric acid are commercially available AG commodity.
It is that the dry graininess waste material of buildings sample of 20g-25g is placed in electromagnetic type mineral breaker that the described waste material of buildings sealing by dry is pulverized, and sealed membrane sealing is pulverized, and crosses 180 μ m sieves, obtains screen underflow.
Beneficial effect of the present invention is: due to the present invention detect adopt before heavy metal zinc in waste material of buildings, copper, lead, chromium content dry, broken, pulverize, clear up and carry out pre-service, effectively heavy metal in waste material of buildings solid is transferred to liquid, crushing process target contaminant loss to be measured is few, digestion process is easy and simple to handle, acid amount consumes few, so measurement result is reliable.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Embodiment 1
(1) get respectively three parts and come from the waste material of buildings 100g that Nanjing steel plant remove on-the-spot, dry 24 hours for 100 ℃; Every part is detected as follows;
(2) adopt jaw crusher to carry out preliminary fragmentation to block waste material of buildings sample, particulate samples after fragmentation is fully mixed to rear tiling, be divided into 4 minutes, choose at random a copy of it and treat subsequent treatment, its quality is 25g;
(3) get the 25g graininess waste material of buildings sample after division in step 2 and be placed in surface plate, 100 ℃ of baking oven inner dryings 1 hour;
(4) get the graininess waste material of buildings sample that 20g is dry and be placed in electromagnetic type mineral breaker, with sealed membrane sealing, pulverize 1 minute, be less than 180 μ m to particle diameter;
(5) particle diameter is less than to the Powdered waste material of buildings sample of 180 μ m and is placed in 100 ℃ of baking oven inner dryings 2 hours to constant weight, take respectively 3 parts of 0.2g powdered samples in teflon crucible, add 9mL now to join chloroazotic acid (hydrochloric acid/nitric acid volume ratio is 3:1), soak 10 minutes, add 1mL40% hydrofluorite, crucible is added a cover to be placed on 180 ℃ of electric hot plates and is heated to dissolution of solid;
(6) in teflon crucible, add 30mL deionized water, on electric hot plate, continue evaporate to dryness to 2-5mL;
(7) treat that crucible is cooling, with 4% nitric acid, be settled to 100mL;
(8) adopt ICP-OES to measure content of beary metal in solution, calculate content of beary metal in waste material of buildings sample, the results are shown in Table 1.
Table 1: embodiment 1 test result
Embodiment 2
(1) get respectively the waste material of buildings that 3 parts of 100g come from certain waste material of buildings stockyard, dry 24 hours for 100 ℃; Every part is detected as follows;
(2) manually block waste material of buildings sample is carried out to preliminary fragmentation, particulate samples after fragmentation is fully mixed to rear tiling, be divided into 4 minutes, choose at random a copy of it and treat subsequent treatment, its quality is 25g;
(3) by the 25g graininess waste material of buildings sample after division in step 2, be placed in surface plate, wherein 2 parts drip Cr, Cu, Pb, Zn solution, dropping add scalar in Table 2, subsequently simultaneously 100 ℃ of baking oven inner dryings 1 hour;
(4) dry graininess waste material of buildings sample is placed in electromagnetic type mineral breaker, with sealed membrane sealing, pulverizes 1 minute, be less than 180 μ m to particle diameter;
(5) particle diameter is less than to the Powdered waste material of buildings sample of 180 μ m and is placed in 100 ℃ of baking oven inner dryings 2 hours to constant weight, for each sample, 3 Duplicate Samples are set, get 0.2g powdered sample in teflon crucible, add 9mL now to join chloroazotic acid (hydrochloric acid/nitric acid volume ratio is 3:1), soak 10 minutes, add 1mL40% hydrofluorite, crucible is added a cover to be placed on 180 ℃ of electric hot plates and is heated to dissolution of solid;
(6) in teflon crucible, add 30mL deionized water, on electric hot plate, continue evaporate to dryness to 2-5mL;
(7) treat that crucible is cooling, with 4% nitric acid, be settled to 100mL;
(8) adopt ICP-OES to measure content of beary metal in solution, in calculating waste material of buildings sample, content of beary metal is in Table 2
Table 2: example 2 test results
By table 1 result, can be found out, because the present invention has done pre-service before waste material of buildings is detected, therefore, reappearance is desirable with stability, and permission standard deviation is all in tolerance interval.As seen from Table 2, in this method, be dried, pulverize, clear up pre-service heavy metal in waste material of buildings solid is transferred to liquid, target contaminant loss is less, recovery of standard addition is greater than 90%, illustrate that this inventive method is good to the pretreating effect of heavy metal detection in waste material of buildings, has guaranteed the reliable of measurement result.
Claims (3)
1. a heavy metal detection method in waste material of buildings, first gets the contaminated by heavy metals waste material of buildings of 100g, carries out inquartation division after pre-service, chooses at random a copy of it and at 100 ℃, dries 1 hour; The waste material of buildings sealing of drying is pulverized 1 minute, be less than 180 μ m to particle diameter; Then take 0.1g-0.3g and be laid on surface plate, be placed in that 100 ℃ of baking ovens are dry dries 2 hours to constant weight; Waste material of buildings powder is placed in teflon crucible again, adds chloroazotic acid 9mL, soak and add 1mL40% hydrofluorite after 10 minutes, crucible is added a cover to be placed on 180 ℃ of electric hot plates and is heated to dissolution of solid; Then in teflon crucible, add 30mL deionized water, continue hot digestion to 2-5mL; Finally, after teflon crucible cool to room temperature, liquid rotating in crucible is moved to plastics volumetric flask, with 4% salpeter solution, be settled to 100mL; Adopt ICP-OES to measure content of beary metal in solution, calculate content of beary metal in waste material of buildings;
After above-mentioned waste material of buildings pre-service, the method for inquartation division is: block waste material of buildings is dried 24 hours in 100 ℃; Adopt jaw crusher or manually block waste material of buildings sample carried out to preliminary fragmentation, the more block waste material of buildings of preliminary fragmentation is fully mixed, tiling, with inquartation division;
Above-mentioned contaminated by heavy metals waste material of buildings is by the waste material of buildings of the pollution of zinc, copper, lead, chromium.
2. heavy metal detection method in a kind of waste material of buildings according to claim 1, is characterized in that: described chloroazotic acid, for now joining chloroazotic acid, measures commercially available AG hydrochloric acid: nitric acid=3:1 volume ratio, mixes.
3. heavy metal detection method in a kind of waste material of buildings according to claim 1, it is characterized in that: it is that the dry graininess waste material of buildings sample of 20g-25g is placed in electromagnetic type mineral breaker that the described waste material of buildings sealing by dry is pulverized, sealed membrane sealing is pulverized, cross 180 μ m sieves, obtain screen underflow.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104713871A (en) * | 2015-02-09 | 2015-06-17 | 南京市产品质量监督检验院 | Detection method of heavy metals Pb, Cd, Cr and Hg in solid surfacing material |
| CN110823988A (en) * | 2018-08-10 | 2020-02-21 | 湖北工业大学 | Method for detecting content of heavy metal cadmium and arsenic in construction waste |
| CN111351779A (en) * | 2018-12-20 | 2020-06-30 | 上海宝钢工业技术服务有限公司 | Method for measuring content of heavy metal cobalt, manganese, nickel, strontium and vanadium in waste oil |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109061046B (en) * | 2018-06-12 | 2022-02-08 | 上海环境卫生工程设计院有限公司 | Method for detecting composition of construction waste |
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| CN110823988A (en) * | 2018-08-10 | 2020-02-21 | 湖北工业大学 | Method for detecting content of heavy metal cadmium and arsenic in construction waste |
| CN111351779A (en) * | 2018-12-20 | 2020-06-30 | 上海宝钢工业技术服务有限公司 | Method for measuring content of heavy metal cobalt, manganese, nickel, strontium and vanadium in waste oil |
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