CN110320298A - The detection method of heavy metal element in a kind of solid waste - Google Patents
The detection method of heavy metal element in a kind of solid waste Download PDFInfo
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- CN110320298A CN110320298A CN201910636911.6A CN201910636911A CN110320298A CN 110320298 A CN110320298 A CN 110320298A CN 201910636911 A CN201910636911 A CN 201910636911A CN 110320298 A CN110320298 A CN 110320298A
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- 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
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- 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
- G01N30/12—Preparation by evaporation
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- 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
- G01N30/14—Preparation by elimination of some components
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- 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
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
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- 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
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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Abstract
The present invention provides a kind of detection method of heavy metal element in solid waste, includes the following steps: S1, crushes solid waste, then solid waste is blended in acid solution, is sufficiently mixed after stirring evenly 10min, and oxidant is added, and is uniformly mixed；S2, solution is placed in ultrasonic extraction 30min in supersonic generator, reaction mixture is filtered to obtain filtrate and filter cake, filter cake is sufficiently washed with deionized water, and cleaning solution and filtrate are merged, then it is evaporated concentration using Rotary Evaporators, after being cooled to room temperature, concentrate is filtered with miillpore filter, then constant volume is diluted, test solution to be detected is obtained；S3, test solution is detected using high performance liquid chromatography, with calculated by peak area content of beary metal.Detection method of the invention is easy to operate, testing cost is lower, and the accuracy detected is also higher.
Description
Technical field
The invention belongs to detection technique fields, and in particular to the detection method of heavy metal element in a kind of solid waste.
Background technique
With the fast development of modern industry, more and more pollutants have been discharged into atmospheric environment, heavy metal-polluted
Dye is that wherein one kind outstanding, heavy metal refer to that atomic density is greater than 5g/cm3Metallic element, mainly include copper, lead, zinc,
Manganese, nickel, vanadium, mercury, tungsten etc., heavy metal can with the strong interaction of generations such as protein, enzyme so that protein and enzyme etc. lose
Activity causes slow poisoning in addition, heavy metal is also possible to accumulate in human organ, thus heavy metal pollution can seriously threaten
The health of the mankind.Contain heterogeneity in the solid wastes such as municipal sludge, river sludge, metallurgical slag, electroplating sludge, soil
With the heavy metal of different content, so detected to the metallic element in solid waste, and the heavy metal in strict control solid waste at
Divide and content is necessary.Thus, it is badly in need of the detection method of a Heavy Metallic Elements.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of detection method of heavy metal element in solid waste,
The detection method is easy to operate, testing cost is lower, and the accuracy detected is also higher.
The present invention provides the following technical solutions:
The detection method of heavy metal element, includes the following steps: in a kind of solid waste
S1, solid waste is crushed, then solid waste is blended in acid solution, be sufficiently mixed after stirring evenly 10min, oxygen is added
Agent is uniformly mixed；
S2, solution is placed in ultrasonic extraction 30min in supersonic generator, then is filtered to obtain by reaction mixture
Filtrate and filter cake sufficiently wash filter cake with deionized water, and cleaning solution and filtrate are merged, and are then carried out using Rotary Evaporators
It is concentrated by evaporation, after being cooled to room temperature, concentrate is filtered with miillpore filter, then dilutes constant volume, obtains confession to be detected
Test sample solution；
S3, test solution is detected using high performance liquid chromatography, with calculated by peak area content of beary metal, chromatography
Condition is chromatographic column: BEN C18 (100 × 2.1nm, 1.7 μm), mobile phase: water-methanol gradient elution, flow velocity 0.5mL/
Min, Detection wavelength 254nm, sample volume are 5 μm.
Preferably, the mesh number that solid waste crushes in S1 step is 200 mesh or less.
Preferably, acid solution described in S1 step is 40% nitric acid solution, and the quality of solid waste sample and nitric acid solution
Mass ratio is 1:3-15.
Preferably, oxidant described in S1 step is hydrogen peroxide solution, and the quality of solid waste sample and hydrogen peroxide solution
Mass ratio is 1:1-3.
Preferably, it is concentrated by evaporation in S2 step to the 1/50-1/10 of original solution volume.
Preferably, the aperture of miillpore filter described in S2 step is 0.22 μm.
Preferably, in S3 step gradient elution program are as follows: when 0-2min, methanol volume fraction be 0%, 2-4min when,
When methanol volume fraction is 5%, 4-6min, when methanol volume fraction is 10%, 6-8min, methanol volume fraction is 15%, 8-
When 10min, methanol volume fraction is 100%.
Preferably, the heavy metal element includes at least one of Hg, Cd, Pb, As, Se, Cr, Ni, Zn, Cu.
The beneficial effects of the present invention are:
The present invention utilizes acid solution and oxidizer treatment solid waste sample, and combines the use of ultrasonic method, facilitates solid waste sample
The dissolution of soluble metal element in product, and help to reduce acid solution dosage；The present invention adopts when handling solid waste sample
The step of with concentration, the concentration of heavy metal is helped to improve, to help to increase the sensitivity detected；The present invention utilizes height
Effect liquid phase chromatogram method detects heavy metal, is the common detecting instrument in laboratory, and easy to operate, testing cost is lower, and
The accuracy of the detection method is also higher.
Specific embodiment
Embodiment 1
S1,3g pedotheque is blended in 40% nitric acid solution of 24g, is sufficiently mixed after stirring evenly 10min, is added
6g hydrogen peroxide solution is uniformly mixed；
S2, solution is placed in ultrasonic extraction 30min in supersonic generator, then is filtered to obtain by reaction mixture
Filtrate and filter cake sufficiently wash filter cake with deionized water, and cleaning solution and filtrate are merged, and are then carried out using Rotary Evaporators
Be concentrated by evaporation, be concentrated by evaporation to the 1/30 of original solution volume, after being cooled to room temperature, by concentrate with 0.22 μm of miillpore filter into
Row filtering, then dilutes constant volume, obtains test solution to be detected；
S3, test solution is detected using high performance liquid chromatography, with calculated by peak area content of beary metal, chromatography
Condition is chromatographic column: BEN C18 (100 × 2.1nm, 1.7 μm), mobile phase: water-methanol gradient elution, flow velocity 0.5mL/
Min, Detection wavelength 254nm, sample volume are 5 μm, wherein the program of gradient elution are as follows: when 0-2min, methanol volume fraction is
When 0%, 2-4min, when methanol volume fraction is 5%, 4-6min, when methanol volume fraction is 10%, 6-8min, methanol volume
When score is 15%, 8-10min, methanol volume fraction is 100%.
Embodiment 2
S1,3g pedotheque is blended in 40% nitric acid solution of 30g, is sufficiently mixed after stirring evenly 10min, is added
9g hydrogen peroxide solution is uniformly mixed；
S2, solution is placed in ultrasonic extraction 30min in supersonic generator, then is filtered to obtain by reaction mixture
Filtrate and filter cake sufficiently wash filter cake with deionized water, and cleaning solution and filtrate are merged, and are then carried out using Rotary Evaporators
Be concentrated by evaporation, be concentrated by evaporation to the 1/20 of original solution volume, after being cooled to room temperature, by concentrate with 0.22 μm of miillpore filter into
Row filtering, then dilutes constant volume, obtains test solution to be detected；
S3, test solution is detected using high performance liquid chromatography, with calculated by peak area content of beary metal, chromatography
Condition is chromatographic column: BEN C18 (100 × 2.1nm, 1.7 μm), mobile phase: water-methanol gradient elution, flow velocity 0.5mL/
Min, Detection wavelength 254nm, sample volume are 5 μm, wherein the program of gradient elution are as follows: when 0-2min, methanol volume fraction is
When 0%, 2-4min, when methanol volume fraction is 5%, 4-6min, when methanol volume fraction is 10%, 6-8min, methanol volume
When score is 15%, 8-10min, methanol volume fraction is 100%.
Embodiment 3
S1,3g pedotheque is blended in 40% nitric acid solution of 24g, is sufficiently mixed after stirring evenly 10min, is added
9g hydrogen peroxide solution is uniformly mixed；
S2, solution is placed in ultrasonic extraction 30min in supersonic generator, then is filtered to obtain by reaction mixture
Filtrate and filter cake sufficiently wash filter cake with deionized water, and cleaning solution and filtrate are merged, and are then carried out using Rotary Evaporators
Be concentrated by evaporation, be concentrated by evaporation to the 1/20 of original solution volume, after being cooled to room temperature, by concentrate with 0.22 μm of miillpore filter into
Row filtering, then dilutes constant volume, obtains test solution to be detected；
S3, test solution is detected using high performance liquid chromatography, with calculated by peak area content of beary metal, chromatography
Condition is chromatographic column: BEN C18 (100 × 2.1nm, 1.7 μm), mobile phase: water-methanol gradient elution, flow velocity 0.5mL/
Min, Detection wavelength 254nm, sample volume are 5 μm, wherein the program of gradient elution are as follows: when 0-2min, methanol volume fraction is
When 100%, 2-4min, when methanol volume fraction is 0%, 4-6min, when methanol volume fraction is 5%, 6-8min, methanol volume
When score is 15%, 8-10min, methanol volume fraction is 100%.
It takes the identical soil in somewhere to carry out the detection of heavy metal element, needs first to crush pedotheque, be sieved, make
The partial size for obtaining soil meets 200 mesh hereinafter, taking the detection method of embodiment 1-3 to be detected, testing result is as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Copper content (%) | 0.29 | 0.28 | 0.31 |
| Lead content (%) | 0.091 | 0.092 | 0.094 |
| Arsenic content (%) | 0.014 | 0.013 | 0.015 |
The reproducibility that can be seen that the detection method from the data of table 1 is preferable, and the accuracy detected is also higher.
These are only the preferred embodiment of the present invention, is not intended to restrict the invention, although with reference to the foregoing embodiments
Invention is explained in detail, for those skilled in the art, still can be to foregoing embodiments institute
The technical solution of record is modified or equivalent replacement of some of the technical features.It is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. the detection method of heavy metal element in a kind of solid waste, which comprises the steps of:
S1, solid waste is crushed, then solid waste is blended in acid solution, be sufficiently mixed after stirring evenly 10min, oxidation is added
Agent is uniformly mixed；
S2, solution is placed in ultrasonic extraction 30min in supersonic generator, is then filtered reaction mixture to obtain filtrate
And filter cake, filter cake is sufficiently washed with deionized water, and cleaning solution and filtrate are merged, is then evaporated using Rotary Evaporators
Concentration, after being cooled to room temperature, concentrate is filtered with miillpore filter, then dilutes constant volume, obtains test sample to be detected
Solution；
S3, test solution is detected using high performance liquid chromatography, with calculated by peak area content of beary metal, chromatographic condition
For chromatographic column: BEN C18 (100 × 2.1nm, 1.7 μm), mobile phase: water-methanol gradient elution, flow velocity 0.5mL/min are examined
Survey wavelength is 254nm, and sample volume is 5 μm.
2. the detection method of heavy metal element in a kind of solid waste according to claim 1, which is characterized in that solid waste powder in S1 step
Broken mesh number is 200 mesh or less.
3. the detection method of heavy metal element in a kind of solid waste according to claim 1, which is characterized in that acid described in S1 step
Solution is 40% nitric acid solution, and the mass ratio of the quality of solid waste sample and nitric acid solution is 1:3-15.
4. the detection method of heavy metal element in a kind of solid waste according to claim 1, which is characterized in that oxygen described in S1 step
Agent is hydrogen peroxide solution, and the quality of solid waste sample and the mass ratio of hydrogen peroxide solution are 1:1-3.
5. the detection method of heavy metal element in a kind of solid waste according to claim 1, which is characterized in that evaporated in S2 step dense
It is reduced to the 1/50-1/10 of original solution volume.
6. the detection method of heavy metal element in a kind of solid waste according to claim 1, which is characterized in that micro- described in S2 step
The aperture of hole filter membrane is 0.22 μm.
7. the detection method of heavy metal element in a kind of solid waste according to claim 1, which is characterized in that gradient is washed in S3 step
De- program are as follows: when 0-2min, when methanol volume fraction is 0%, 2-4min, when methanol volume fraction is 5%, 4-6min, first
When alcohol volume fraction is 10%, 6-8min, when methanol volume fraction is 15%, 8-10min, methanol volume fraction is 100%.
8. the detection method of heavy metal element in a kind of solid waste according to claim 7, which is characterized in that the heavy metal element
Including at least one of Hg, Cd, Pb, As, Se, Cr, Ni, Zn, Cu.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220692A (en) * | 2020-01-16 | 2020-06-02 | 通标标准技术服务（天津）有限公司 | Method for detecting content of heavy metal in food contact material |
| CN115598287A (en) * | 2022-12-14 | 2023-01-13 | 苏州星翰新材料科技有限公司（Cn） | Method for detecting copper content in conductive paste |
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| 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 |
| CN105928926A (en) * | 2016-04-19 | 2016-09-07 | 攀钢集团研究院有限公司 | Sample preparation method and detection method for water-soluble heavy metal elements in solid waste |
| CN106526011A (en) * | 2016-11-03 | 2017-03-22 | 百奥森（江苏）食品安全科技有限公司 | Detection method for heavy metal |
| CN107167361A (en) * | 2017-07-07 | 2017-09-15 | 苏州汉宣检测科技有限公司 | A kind of heavy metal in soil content analysis method |
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2019
- 2019-07-15 CN CN201910636911.6A patent/CN110320298A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374629A (en) * | 2014-11-17 | 2015-02-25 | 渤海大学 | Ultrasonic extraction method of heavy metal elements in vegetables |
| 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 |
| CN105928926A (en) * | 2016-04-19 | 2016-09-07 | 攀钢集团研究院有限公司 | Sample preparation method and detection method for water-soluble heavy metal elements in solid waste |
| CN106526011A (en) * | 2016-11-03 | 2017-03-22 | 百奥森（江苏）食品安全科技有限公司 | Detection method for heavy metal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220692A (en) * | 2020-01-16 | 2020-06-02 | 通标标准技术服务（天津）有限公司 | Method for detecting content of heavy metal in food contact material |
| CN115598287A (en) * | 2022-12-14 | 2023-01-13 | 苏州星翰新材料科技有限公司（Cn） | Method for detecting copper content in conductive paste |
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Application publication date: 20191011 |