CN104034720B - Heavy metal detection method in a kind of waste material of buildings - Google Patents
Heavy metal detection method in a kind of waste material of buildings Download PDFInfo
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- CN104034720B CN104034720B CN201410245673.3A CN201410245673A CN104034720B CN 104034720 B CN104034720 B CN 104034720B CN 201410245673 A CN201410245673 A CN 201410245673A CN 104034720 B CN104034720 B CN 104034720B
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Abstract
The present invention relates to heavy metal detection method in a kind of waste material of buildings.First take the contaminated by heavy metals waste material of buildings of 100g, carry out quartering division after pretreatment, randomly select a copy of it and dry 1 hour at 100 DEG C;Dry waste material of buildings sealing powder is broken to particle diameter less than 180 μm;Then weigh 0.1g 0.3g to be laid on surface plate, be placed in 100 DEG C of baking ovens and dry 2 hours to constant weight;Being placed in politef crucible by waste material of buildings powder, add chloroazotic acid 9mL, add 1mL40% Fluohydric acid. after soaking 10 minutes, crucible is added a cover to be placed on 180 DEG C of electric hot plates and is heated to solid dissolving;Then in politef crucible, add 30mL deionized water, continuation heating steaming and decocting to 2 5mL;Finally after politef crucible is cooled to room temperature, liquid in crucible is transferred to plastics volumetric flask, is settled to 100mL with 4% salpeter solution;ICP OES is used to measure content of beary metal in solution.The present invention measures the most 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 inspection in waste material of buildings
Survey technology field.
Background technology
Along with developing rapidly of China's economy and quickly propelling of urbanization process, removal, reorganization and expansion and New any
Mesh produces a large amount of waste material of buildings, it is estimated that the annual building waste that produces is about 2,400,000,000 tons, including in a large number
The contaminated waste material of buildings that chemical industry, metallurgy, light industry, the removal of processing enterprise or reconstruction produce.Detection building is useless
Content of beary metal in thing, differentiates common buildings refuse and contaminated waste material of buildings, the pollution shape of investigation waste material of buildings
Condition, is beneficial to the further harmless resource utilization of waste material of buildings.But waste material of buildings character is special, need before detection into
The pretreatment that row is certain.Such as concrete, fragment of brick class waste material of buildings quality is hard, containing a large amount of silicon dioxide etc.
Material, the dust of crushing process is revealed and digestion process the most all can cause last mensuration inaccurate.
Lack the standard method that waste material of buildings content of beary metal measures at present both at home and abroad, literature research uses soil more
The digestion procedure of heavy metal in earth, the method acid consumption is big, clears up as heavy metal in waste material of buildings, and it is accurate
Property quantitatively judge, in a word, the accurate method of content of beary metal detection in so far there are no waste material of buildings, also lack
The weary recovery of standard addition checking about content of beary metal detection in waste material of buildings.
Summary of the invention
It is an object of the invention to provide a kind of method of heavy metal analysis in waste material of buildings, be particularly used for detection and build
Build zinc in refuse, copper, lead, the processing method of chromium content.
For reaching above-mentioned purpose, the present invention is directed to content of beary metal detection feature in waste material of buildings, the most successively according to dry
Dry, crush, pulverize, clear up and carry out pretreatment, then constant volume, measure and be calculated a huge sum of money in waste material of buildings
Belong to content.Specifically comprise the following steps that
First take the contaminated by heavy metals waste material of buildings of 100g, carry out quartering division after pretreatment, randomly select
A copy of it is dried 1 hour at 100 DEG C;The waste material of buildings dried is sealed and pulverizes 1 minute, little to particle diameter
In 180 μm;Then weigh 0.1g-0.3g to be laid on surface plate, be placed in 100 DEG C of baking ovens and be dried drying 2
Hour to constant weight;Again waste material of buildings powder is placed in politef crucible, adds chloroazotic acid 9mL, soak
Adding 1mL40% Fluohydric acid. after 10 minutes, crucible is added a cover to be placed on 180 DEG C of electric hot plates and is heated to solid dissolving;
Then in politef crucible, add 30mL deionized water, continuation heating steaming and decocting to 2-5mL;Finally treat
After politef crucible is cooled to room temperature, liquid in crucible is transferred to plastics volumetric flask, molten with 4% nitric acid
Liquid is settled to 100mL;Use ICP-OES to measure content of beary metal in solution, calculate a huge sum of money in waste material of buildings
Belong to content;
After above-mentioned waste material of buildings sample pretreatment, the method for quartering division is: by the baking of 100 DEG C of waste material of buildings sample
Dry 24 hours;Use jaw crusher or manually block waste material of buildings sample tentatively crushed, then will just
The block waste material of buildings that step crushes is sufficiently mixed uniformly, and tiling, with quartering division;
Above-mentioned contaminated by heavy metals waste material of buildings is by zinc, copper, lead, the waste material of buildings of pollution of chromium.
Described chloroazotic acid, for now to join chloroazotic acid, measures hydrochloric acid: nitric acid=3:1 volume ratio, mix homogeneously.Used
Hydrochloric acid and nitric acid are commercially available AG commodity.
Described dry waste material of buildings sealing being pulverized is the graininess waste material of buildings sample being dried by 20g-25g
Product are placed in electromagnetic type mineral breaker, and sealed membrane seals to be pulverized, and cross 180 μm sieves, obtain siftage.
The beneficial effects of the present invention is: owing to the present invention detects heavy metal zinc in waste material of buildings, copper, lead, chromium
Use before content and be dried, crush, pulverize, clear up and carry out pretreatment, effectively by heavy metal in waste material of buildings solid
Being transferred to liquid, the loss of crushing process target contaminant to be measured is few, and digestion process is easy and simple to handle, and acid amount consumes few,
Therefore measurement result is reliable.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the present invention.
Detailed description of the invention
Embodiment 1
(1) take three parts respectively and come from the waste material of buildings 100g that the removal of Nanjing steel plant is on-the-spot, 100 DEG C of drying
24 hours;Every part is detected as follows;
(2) use jaw crusher that block waste material of buildings sample is tentatively crushed, will broken rear granular
Product tile after being sufficiently mixed uniformly, are divided into 4 points, randomly select a copy of it and treat subsequent treatment, its quality
For 25g;
(3) take in step 2 the 25g graininess waste material of buildings sample after division to be placed in surface plate, 100 DEG C of bakings
It is dried 1 hour in case;
(4) take the graininess waste material of buildings sample that 20g is dried to be placed in electromagnetic type mineral breaker, with sealing
Film phonograph seal is pulverized 1 minute, to particle diameter less than 180 μm;
(5) it is dried 2 hours in particle diameter being placed in 100 DEG C of baking ovens less than 180 μm powder waste material of buildings samples
To constant weight, weigh 3 parts of 0.2g powder samples respectively in politef crucible, add 9mL and now join chloroazotic acid
(hydrochloric acid/nitric acid volume ratio is 3:1), soaks 10 minutes, adds 1mL40% Fluohydric acid., and crucible is added a cover and put
On 180 DEG C of electric hot plates, it is heated to solid dissolve;
(6) in politef crucible, add 30mL deionized water, continue to be evaporated on electric hot plate to
2-5mL;
(7) treat that crucible cools down, be settled to 100mL with 4% nitric acid;
(8) use ICP-OES to measure content of beary metal in solution, calculate heavy metal in waste material of buildings sample and contain
Amount, the results are shown in Table 1.
Table 1: embodiment 1 test result
Embodiment 2
(1) take 3 parts of 100g respectively and come from the waste material of buildings in certain waste material of buildings stockyard, dry 24 hours for 100 DEG C;
Every part is detected as follows;
(2) manually block waste material of buildings sample is tentatively crushed, broken rear particulate samples is sufficiently mixed all
After even, tiling, is divided into 4 points, randomly selects a copy of it and treat subsequent treatment, and its quality is 25g;
(3) by the 25g graininess waste material of buildings sample after division in step 2, it is placed in surface plate, wherein 2 parts
Dropping Cr, Cu, Pb, Zn solution, the scalar that adds of dropping is shown in Table 2, simultaneously dry in 100 DEG C of baking ovens subsequently
Dry 1 hour;
(4) dry graininess waste material of buildings sample is placed in electromagnetic type mineral breaker, seals with sealed membrane
Pulverize 1 minute, to particle diameter less than 180 μm;
(5) 2 hours it are dried in particle diameter being placed in 100 DEG C of baking ovens less than 180 μm powder waste material of buildings samples extremely
Constant weight, arranges 3 Duplicate Samples for each sample, takes 0.2g powder sample in politef crucible,
Add 9mL and now join chloroazotic acid (hydrochloric acid/nitric acid volume ratio is 3:1), soak 10 minutes, add 1mL40% hydrogen
Fluoric acid, crucible is added a cover to be placed on 180 DEG C of electric hot plates and is heated to solid dissolving;
(6) in politef crucible, add 30mL deionized water, continue to be evaporated on electric hot plate to
2-5mL;
(7) treat that crucible cools down, be settled to 100mL with 4% nitric acid;
(8) use ICP-OES to measure content of beary metal in solution, calculate heavy metal in waste material of buildings sample and contain
Amount is shown in Table 2
Table 2: example 2 test result
Be can be seen that by table 1 result, before waste material of buildings being detected due to the present invention, done pretreatment, therefore, reappear
Property preferable with stability, it is allowed to standard deviation is all in tolerance interval.As seen from Table 2, in this method
Being dried, pulverize, clear up pretreatment heavy metal in waste material of buildings solid is transferred to liquid, target contaminant loses
Less, recovery of standard addition is more than 90%, illustrates that this inventive method is to the pretreatment of heavy metal analysis in waste material of buildings
Effective, it is ensured that measurement result reliable.
Claims (3)
1. a heavy metal detection method in waste material of buildings, first takes the contaminated by heavy metals waste material of buildings of 100g,
Carry out quartering division after pretreatment, randomly select a copy of it and dry 1 hour at 100 DEG C;By dry
Waste material of buildings seals to be pulverized 1 minute, to particle diameter less than 180 μm;Then weigh 0.1g-0.3g and be laid in surface
On ware, it is placed in 100 DEG C of baking ovens to be dried and dries 2 hours to constant weight;Again waste material of buildings powder is placed in polytetrafluoro
In ethylene crucible, adding chloroazotic acid 9mL, add 1mL40% Fluohydric acid. after soaking 10 minutes, crucible is added a cover and is put
On 180 DEG C of electric hot plates, it is heated to solid dissolve;Then in politef crucible, add 30mL deionization
Water, continuation heating steaming and decocting to 2-5mL;Finally after politef crucible is cooled to room temperature, by liquid in crucible
Body is transferred to plastics volumetric flask, is settled to 100mL with 4% salpeter solution;ICP-OES is used to measure in solution
Content of beary metal, calculates content of beary metal in waste material of buildings;
After above-mentioned waste material of buildings pretreatment, the method for quartering division is: by bulk waste material of buildings in 100 DEG C of drying
24 hours;Use jaw crusher or manually block waste material of buildings sample tentatively crushed, then will be preliminary
Broken block waste material of buildings is sufficiently mixed uniformly, and tiling, with quartering division;
Above-mentioned contaminated by heavy metals waste material of buildings is by zinc, copper, lead, the waste material of buildings of pollution of chromium.
Heavy metal detection method in a kind of waste material of buildings, it is characterised in that: institute
State chloroazotic acid for now to join chloroazotic acid, measure commercially available AG hydrochloric acid: nitric acid=3:1 volume ratio, mixing.
Heavy metal detection method in a kind of waste material of buildings, it is characterised in that: institute
Dry waste material of buildings sealing being pulverized of stating is that the graininess waste material of buildings sample being dried by 20g-25g is placed in electricity
In magnetic-type mineral breaker, sealed membrane seals to be pulverized, and crosses 180 μm sieves, obtains siftage.
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Cited By (1)
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CN109061046A (en) * | 2018-06-12 | 2018-12-21 | 上海环境卫生工程设计院有限公司 | A method of detection building waste composition |
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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 |
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