CN106526011A - Detection method for heavy metal - Google Patents
Detection method for heavy metal Download PDFInfo
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- CN106526011A CN106526011A CN201610949613.9A CN201610949613A CN106526011A CN 106526011 A CN106526011 A CN 106526011A CN 201610949613 A CN201610949613 A CN 201610949613A CN 106526011 A CN106526011 A CN 106526011A
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- heavy metal
- detection method
- citric acid
- sample
- disodiumedetate
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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
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- Chemical & Material Sciences (AREA)
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- Biochemistry (AREA)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a detection method for heavy metal. The method comprises the steps of weighing and taking 0.8-1.2 g sample to be tested and making it through a 100-mesh sieve, adding the sample to be tested into a beaker, and adding deionized water or lye and stirring evenly; adding citric acid and ethylene diamine tetraacetic acid disodium in proportion, and performing stirring; conducting filtering, and taking a filtrate to obtain a blank solution; adopting a super efficient liquid chromatography to conduct quantitative determination on the obtained test solution. The detection method for heavy metal is efficient and simple in operation, can detect out super-low-concentration heavy metal, and increases the sensitivity of sample determination; the method is low in detection cost, can be used for determining multiple heavy metal elements, does not need to solely conduct pretreatment on every heavy metal element, and reduces workload. The detection method for heavy metal has high detection efficiency, and has the advantages of being good in recovery rate, high in accuracy, fast in processing speed, simple in operation, wide in range of application and the like.
Description
Technical field
The present invention relates to technical field of analysis and detection, the specifically detection method of heavy metal species.
Background technology
Heavy metal refers to that atomic density is more than 5g/cm3Metallic element, there are about 45 kinds, such as copper, lead, zinc, good fortune, manganese, ferrum, brill,
Nickel, vanadium, admire, hydrargyrum, tungsten, aluminum, gold, silver etc..Although the heavy metals such as manganese, copper, zinc are the trace element required for vital movement,
Not vital movement institute is required for most of heavy metal such as lead, hydrargyrum etc., and all heavy metals all have to human body more than finite concentration
Poison.With the development of the expansion and large-scale industry in city, heavy metal pollution mouth benefit present in air, soil, water environment increases
Plus.Heavy metal pollution is one of subject matter of water pollution, mining, metal smelt, chemical production wastewater, applying pesticides
Fertilizer and the artificial pollution such as house refuse, and the natural factor such as geologic erosion, air slaking can cause heavy metal to be entered in a variety of manners
Enter soil.As heavy metal has that toxicity is big, is difficult in the environment to be metabolized, is easily bioaccumulation and has biological amplification etc.
Feature so that heavy metal pollution seriously threatens human health.Therefore, the monitoring and control of content of beary metal oneself become and be related to ring
The major issue that border protection, sustainable development and Living consumption are improved.
The content of the invention
It is an object of the invention to provide a kind of response rate is good, precision is high, processing speed is fast, model easy to operate, applicable
The detection method of wide heavy metal is enclosed, to solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme：
The detection method of one heavy metal species, comprises the following steps：
1）The testing sample for weighing 0.8-1.2g crosses 100 mesh sieves, in adding beaker, adds deionized water or alkali liquor to stir；
2）Citric acid and disodiumedetate are proportionally added into, and are stirred 25-40min；Using citric acid：Second two
The mass ratio of amine tetraacethyl disodium is 1：1-5；
3）By step 2）In sample filtering, take filtrate and obtain final product need testing solution；
4）Prepare blank solution：Deionized water or alkali liquor are measured, citric acid and disodiumedetate is proportionally added into, is gone forward side by side
Row stirring 25-40min；Using citric acid：The mass ratio of disodiumedetate is 1：1-5；Filter, take filtrate, obtain final product
Blank solution；
5）Quantitative determination：Gained need testing solution is quantitative determined using ultra-performance liquid chromatography.
As further scheme of the invention：Alkali liquor is the mixture of sodium hydroxide and potassium hydroxide, hydroxide ion
Concentration is 0.3-2mol/L.
As further scheme of the invention：Chromatographic column used by ultra-performance liquid chromatography is ACQUITYUPLC BEH
C18, chromatographic column specification is 1.7 μm, 2.1 × 50mm, and mobile phase is water-methanol gradient elution, and the time is respectively 0,1 .1,2,3,
When 4,7,8,8.5,11 minutes, the mass percent of water and methanol is respectively 100：0,100：0,98：2,90：10,85：15,0：
100,0：100,100：0,100：0, Detection wavelength 254nm, flow velocity 0.5m L min-1, 5 μ L of sample size, with external standard method with peak face
Product is calculated.
Compared with prior art, the invention has the beneficial effects as follows：
The heavy metal analysis pre-treating method of the present invention is efficient, easy to operate, can detect that the heavy metal of super low concentration, it is to avoid
The loss and air pollution of heavy metal element；Increased the sensitivity of sample determination.The pre-treatment raw material sources that the present invention is used
Extensively, it is cheap, therefore testing cost is low.Can be used for the measure of detection device for multi metallic elements, it is not necessary to per Heavy Metallic Elements list
The pretreatment of sample is solely carried out, workload is reduced.The present invention is sensitiveer on detection content of beary metal, with higher inspection
Efficiency is surveyed, has the advantages that the response rate is good, precision is high, processing speed is fast, easy to operate, applied widely.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment obtained under the premise of creative work is not made by those of ordinary skill in the art, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, the detection method of heavy metal species is comprised the following steps：
1）The testing sample for weighing 0.8g crosses 100 mesh sieves, in adding beaker, adds deionized water to stir.2）In proportion plus
Enter citric acid and disodiumedetate, and be stirred 25min；Using citric acid：The matter of disodiumedetate
Amount is than being 1：1；
3）By step 2）In sample filtering, take filtrate and obtain final product need testing solution；
4）Prepare blank solution：Deionized water is measured, citric acid and disodiumedetate is proportionally added into, and is stirred
25min；Using citric acid：The mass ratio of disodiumedetate is 1：1；Filter, take filtrate, obtain final product blank solution；
5）Quantitative determination：Gained need testing solution is quantitative determined using ultra-performance liquid chromatography.Ultra high efficiency liquid phase color
Chromatographic column used by spectrometry is ACQUITYUPLC BEH C18, chromatographic column specification be 1.7 μm, 2.1 × 50mm, mobile phase be water-
Methanol elution gradient, time are respectively 0,1 .1, the mass percent difference of water and methanol when 2,3,4,7,8,8.5,11 minutes
For 100：0,100：0,98：2,90：10,85：15,0：100,0：100,100：0,100：0, Detection wavelength 254nm, flow velocity 0.5m
L·min-1, 5 μ L of sample size, with external standard method with calculated by peak area.
Embodiment 2
In the embodiment of the present invention, the detection method of heavy metal species is comprised the following steps：
1）The testing sample for weighing 1.2g crosses 100 mesh sieves, in adding beaker, adds alkali liquor to stir.Alkali liquor is sodium hydroxide
With the mixture of potassium hydroxide, the concentration of hydroxide ion is 0.3mol/L；
2）Citric acid and disodiumedetate are proportionally added into, and are stirred 40min；Using citric acid：Ethylenediamine
The mass ratio of tetraacethyl disodium is 1：5；
3）By step 2）In sample filtering, take filtrate and obtain final product need testing solution；
4）Prepare blank solution：Deionized water or alkali liquor are measured, citric acid and disodiumedetate is proportionally added into, is gone forward side by side
Row stirring 40min；Using citric acid：The mass ratio of disodiumedetate is 1：5；Filter, take filtrate, obtain final product blank molten
Liquid；
5）Quantitative determination：Gained need testing solution is quantitative determined using ultra-performance liquid chromatography.Ultra high efficiency liquid phase color
Chromatographic column used by spectrometry is ACQUITYUPLC BEH C18, chromatographic column specification be 1.7 μm, 2.1 × 50mm, mobile phase be water-
Methanol elution gradient, time are respectively 0,1 .1, the mass percent difference of water and methanol when 2,3,4,7,8,8.5,11 minutes
For 100：0,100：0,98：2,90：10,85：15,0：100,0：100,100：0,100：0, Detection wavelength 254nm, flow velocity 0.5m
L·min-1, 5 μ L of sample size, with external standard method with calculated by peak area.
Embodiment 3
In the embodiment of the present invention, the detection method of heavy metal species is comprised the following steps：
1）The testing sample for weighing 1g crosses 100 mesh sieves, in adding beaker, adds alkali liquor to stir.Alkali liquor be sodium hydroxide with
The mixture of potassium hydroxide, the concentration of hydroxide ion is 2mol/L；
2）Citric acid and disodiumedetate are proportionally added into, and are stirred 30min；Using citric acid：Ethylenediamine
The mass ratio of tetraacethyl disodium is 1：3；
3）By step 2）In sample filtering, take filtrate and obtain final product need testing solution；
4）Prepare blank solution：Deionized water or alkali liquor are measured, citric acid and disodiumedetate is proportionally added into, is gone forward side by side
Row stirring 30min；Using citric acid：The mass ratio of disodiumedetate is 1：3；Filter, take filtrate, obtain final product blank molten
Liquid；
5）Quantitative determination：Gained need testing solution is quantitative determined using ultra-performance liquid chromatography.Ultra high efficiency liquid phase color
Chromatographic column used by spectrometry is ACQUITYUPLC BEH C18, chromatographic column specification be 1.7 μm, 2.1 × 50mm, mobile phase be water-
Methanol elution gradient, time are respectively 0,1 .1, the mass percent difference of water and methanol when 2,3,4,7,8,8.5,11 minutes
For 100：0,100：0,98：2,90：10,85：15,0：100,0：100,100：0,100：0, Detection wavelength 254nm, flow velocity 0.5m
L·min-1, 5 μ L of sample size, with external standard method with calculated by peak area.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of description is only that those skilled in the art should for clarity
Using description as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art
Understandable other embodiment.
Claims (3)
1. the detection method of heavy metal species, it is characterised in that comprise the following steps：
1）The testing sample for weighing 0.8-1.2g crosses 100 mesh sieves, in adding beaker, adds deionized water or alkali liquor to stir；
2）Citric acid and disodiumedetate are proportionally added into, and are stirred 25-40min；Using citric acid：Second two
The mass ratio of amine tetraacethyl disodium is 1：1-5；
3）By step 2）In sample filtering, take filtrate and obtain final product need testing solution；
4）Prepare blank solution：Deionized water or alkali liquor are measured, citric acid and disodiumedetate is proportionally added into, is gone forward side by side
Row stirring 25-40min；Using citric acid：The mass ratio of disodiumedetate is 1：1-5；Filter, take filtrate, obtain final product
Blank solution；
5）Quantitative determination：Gained need testing solution is quantitative determined using ultra-performance liquid chromatography.
2. the detection method of heavy metal according to claim 1, it is characterised in that alkali liquor is sodium hydroxide and potassium hydroxide
Mixture, the concentration of hydroxide ion is 0.3-2mol/L.
3. the detection method of heavy metal according to claim 1, it is characterised in that the color used by ultra-performance liquid chromatography
Spectrum post is ACQUITYUPLC BEH C18, chromatographic column specification is 1.7 μm, and 2.1 × 50mm, mobile phase are water-methanol gradient elution,
Time is respectively 0,1 .1, and when 2,3,4,7,8,8.5,11 minutes, the mass percent of water and methanol is respectively 100：0,100：0,
98：2,90：10,85：15,0：100,0：100,100：0,100：0, Detection wavelength 254nm, flow velocity 0.5m L min-1, sample introduction
5 μ L are measured, with external standard method with calculated by peak area.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610949613.9A CN106526011A (en) | 2016-11-03 | 2016-11-03 | Detection method for heavy metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610949613.9A CN106526011A (en) | 2016-11-03 | 2016-11-03 | Detection method for heavy metal |
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| Publication Number | Publication Date |
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| CN106526011A true CN106526011A (en) | 2017-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610949613.9A Pending CN106526011A (en) | 2016-11-03 | 2016-11-03 | Detection method for heavy metal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110320298A (en) * | 2019-07-15 | 2019-10-11 | 江苏天宇检测技术有限公司 | The detection method of heavy metal element in a kind of solid waste |
| CN113861018A (en) * | 2021-11-01 | 2021-12-31 | 莱芜泰禾生化有限公司 | Purification treatment method of citric acid mother liquor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539425A (en) * | 2011-12-30 | 2012-07-04 | 中国计量学院 | Raid detection method for heavy metal lead in tea leaves |
| CN102661887A (en) * | 2012-04-24 | 2012-09-12 | 红河学院 | Method for removing micro heavy metal in reagent solution |
| CN104596952A (en) * | 2013-10-31 | 2015-05-06 | 大连大公环境检测有限公司 | Method for detecting content of heavy metals in garbage landfill soil |
| 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 |
-
2016
- 2016-11-03 CN CN201610949613.9A patent/CN106526011A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539425A (en) * | 2011-12-30 | 2012-07-04 | 中国计量学院 | Raid detection method for heavy metal lead in tea leaves |
| CN102661887A (en) * | 2012-04-24 | 2012-09-12 | 红河学院 | Method for removing micro heavy metal in reagent solution |
| CN104596952A (en) * | 2013-10-31 | 2015-05-06 | 大连大公环境检测有限公司 | Method for detecting content of heavy metals in garbage landfill soil |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 尹雪等: ""EDTA 与柠檬酸复配洗涤修复多重金属污染土壤效果研究", 《环境科学》 * |
| 张晏溧等: "EDTA 与柠檬酸释放土壤中 Cd、Pb 的影响研究", 《环境科学与管理》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110320298A (en) * | 2019-07-15 | 2019-10-11 | 江苏天宇检测技术有限公司 | The detection method of heavy metal element in a kind of solid waste |
| CN113861018A (en) * | 2021-11-01 | 2021-12-31 | 莱芜泰禾生化有限公司 | Purification treatment method of citric acid mother liquor |
| CN113861018B (en) * | 2021-11-01 | 2024-02-20 | 莱芜泰禾生化有限公司 | Purification treatment method of citric acid mother liquor |
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Application publication date: 20170322 |
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