CN110346444A - The extracting method of heavy metal available state in a kind of yellow moist soil - Google Patents
The extracting method of heavy metal available state in a kind of yellow moist soil Download PDFInfo
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- CN110346444A CN110346444A CN201910597774.XA CN201910597774A CN110346444A CN 110346444 A CN110346444 A CN 110346444A CN 201910597774 A CN201910597774 A CN 201910597774A CN 110346444 A CN110346444 A CN 110346444A
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Abstract
The present invention provides a kind of extracting methods of heavy metal available state in yellow moist soil, the described method comprises the following steps: (1) mixing extractant and soil and be uniformly dispersed, obtain extraction system；Wherein, the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2The concentration of EDTA is 0.05-0.2mol/L, and the pH of mixed aqueous solution is 6-8；(2) it is vortexed to extraction system or shakes extraction；(3) it is separated by solid-liquid separation, collects extracting solution.Extracting method of the invention can more effectively extract the heavy metal available state in yellow moist soil, the recovery rate for extracting the heavy metal available state in obtained extracting solution is high, accuracy, the stability of extraction are good, and method is simple, and the parameter of selected extractant and extractant can preferably avoid non-effective state heavy metal from being extracted in extracting solution, can preferably avoid the influence of heavy metal pollution risk of the non-effective state heavy metal in evaluation soil.
Description
Technical field
The invention belongs to method of environmental monitoring fields, and in particular to the extraction side of heavy metal available state in a kind of yellow moist soil
Method.
Background technique
Heavy metal pollution of soil has the characteristics that chronicity, cumulative bad, latency and irreversible, to soil, underground water, micro-
The ecosystems such as biology, plant, which constitute, to be seriously threatened, and is that agricultural sustainable development and environmental quality improve face important and ask
Topic.The eco-toxicity of heavy metal is not only related to total amount, be also largely dependent upon its existing forms in the soil and
Its combination.Water-soluble state, exchangeable species can be classified as, in conjunction with carbonate according to heavy metal and the combining form of surrounding medium
State, six class of ferrimanganic reference state, organic sulfide state and residual form, wherein water-soluble state, exchangeable species and the direct shadow of carbonate combine state
The environmental behaviour for ringing heavy metal, determines biological effectiveness and environmental risk degree, and therefore, this part is commonly known as " effectively
State ".
For the risk of the heavy metal pollution in accurate evaluation soil, a kind of extracting method of heavy metal in soil is needed, but
Be presently, there are extracting method in, cannot there are the non-effective state of heavy metal in the heavy metal that single-stage extraction method is extracted
Avoid the influence of the risk of heavy metal pollution of the non-effective state of heavy metal in evaluation soil.
Summary of the invention
Heavy metal in a kind of yellow moist soil is provided it is an object of the invention to overcome in place of the shortcomings of the prior art to be had
Imitate the extracting method of state.
To achieve the above object, the technical scheme adopted by the invention is as follows in a kind of yellow moist soil heavy metal available state extraction side
Method the described method comprises the following steps:
(1) extractant and soil are mixed and is uniformly dispersed, obtain extraction system；
Wherein, the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's is dense
Degree is 0.05-0.2mol/L, and the pH of mixed aqueous solution is 6-8；
(2) it is vortexed to extraction system or shakes extraction；
(3) it is separated by solid-liquid separation, collects extracting solution；
The wherein heavy metal are as follows: at least one of 3 heavy metal species of cadmium (Cd), zinc (Zn) and arsenic (As) heavy metal is appointed
Meaning combination.
Extracting method of the invention can more effectively extract the heavy metal available state in yellow moist soil, the extraction extracted
The recovery rate of heavy metal available state in liquid is high, and accuracy, the stability of extraction are good, and method is simple, and selected extraction
The parameter of agent and extractant can preferably avoid non-effective state heavy metal from being extracted in extracting solution, can preferably avoid non-effective
The influence of heavy metal pollution risk of the state heavy metal in evaluation soil.
Preferably, the pH of the mixed aqueous solution is 6-7.
When the pH of the mixed aqueous solution as extractant is 6-7, when the recovery rate of heavy metal available state relative to pH is 8
It is higher.
Preferably, Na in the mixed aqueous solution2The concentration of EDTA is 0.05-0.1mol/L.
Preferably, the amount ratio of the soil and extractant are as follows: 1:10g/mL-1:40g/mL.
Preferably, the amount ratio of the soil and extractant are as follows: 1:20g/mL.
Preferably, in step (2), to extract system frequency of oscillation be 200rpm horizontal oscillations shaking table extract 0.5h with
On.
Preferably, in step (2), 0.5h-8h is extracted for 200rpm horizontal oscillations shaking table in frequency of oscillation to the system of extraction.
Preferably, Na in the mixed aqueous solution2The concentration of EDTA is 0.05mol/L.
Preferably, the pH of the mixed aqueous solution is 6.
Preferably, it is uniformly dispersed after extractant and soil mixing by swirl mixing device concussion in step (1)；Step (2)
Middle holding extraction system extracts at 25 ± 2 DEG C.
The present invention also provides a kind of detection methods of heavy metal available state in yellow moist soil, the described method comprises the following steps:
(a) heavy metal available state in yellow moist soil is extracted by such as any of the above-described the method and obtains extracting solution；
(b) it by extracting solution loading described in step (a), is quantified with ICP-MS.
This method is avoided since the heavy metal in the extracting solution that extracts in extraction process is heavy metal available state
The interference of the non-effective state of heavy metal, being capable of the more acurrate heavy metal pollution risk objectively evaluated in soil.
The beneficial effects of the present invention are: the present invention provides a kind of extracting methods of heavy metal available state in moisture soil, originally
The extracting method of invention can more effectively extract the heavy metal available state in yellow moist soil, the huge sum of money in extracting solution extracted
The recovery rate for belonging to available state is high, and accuracy, the stability of extraction are good, and method is simple, can handle batch samples simultaneously, side
Just for evaluating the influence of heavy metal pollution risk in soil in environmental analysis, and selected extractant and extractant
Parameter can preferably avoid non-effective state heavy metal from being extracted in extracting solution, and non-effective state heavy metal can preferably be avoided to comment
The influence of heavy metal pollution risk in valence soil.
Detailed description of the invention
Fig. 1 is influence diagram of the concentration to extraction effect of the extractant of the extracting method of the embodiment of the present invention.
The extractant and soil ratio that Fig. 2 is the extracting method of the embodiment of the present invention are to the influence diagram of extraction effect.
Fig. 3 is influence diagram of the extraction time to extraction effect of the extracting method of the embodiment of the present invention.
Fig. 4 is influence diagram of the pH to extraction effect of the extractant of the extracting method of the embodiment of the present invention.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the method includes following
Step:
(1) it is uniformly dispersed after mixing the extractant of 20mL and 1g soil with swirl mixing device oscillation 30s, obtains extracting body
System；
Wherein, the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's is dense
Degree is 0.05mol/L, and the pH of mixed aqueous solution is 7；
(2) by extraction system be placed in temperature be 25 ± 2 DEG C, frequency of oscillation be 200rpm horizontal oscillations shaking table extract 2h；
(3) it is separated by solid-liquid separation, collects extracting solution；
The wherein heavy metal are as follows: cadmium, zinc, 3 heavy metal species of arsenic.
Embodiment 2
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the present embodiment and embodiment
1 unique difference are as follows: Na in mixed aqueous solution2The concentration of EDTA is 0.1mol/L.
Embodiment 3
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the present embodiment and embodiment
1 unique difference are as follows: Na in mixed aqueous solution2The concentration of EDTA is 0.2mol/L.
Comparative example 1
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
1 unique difference are as follows: Na in mixed aqueous solution2The concentration of EDTA is 0.005mol/L.
Comparative example 2
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
1 unique difference are as follows: Na in mixed aqueous solution2The concentration of EDTA is 0.01mol/L.
Embodiment 4
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the method includes following
Step:
(1) it is uniformly dispersed after mixing the extractant of 20mL and 1g soil with swirl mixing device oscillation 30s, obtains extracting body
System；
Wherein, the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's is dense
Degree is 0.05mol/L, and the pH of mixed aqueous solution is 7；
(2) by extraction system be placed in temperature be 25 ± 2 DEG C, frequency of oscillation be 200rpm horizontal oscillations shaking table extract 0.5h；
(3) it is separated by solid-liquid separation, collects extracting solution；
The wherein heavy metal are as follows: cadmium, zinc, 3 heavy metal species of arsenic.
Embodiment 5
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the present embodiment and embodiment
4 unique difference are as follows: swirl mixing device oscillation 30s is uniformly dispersed after mixing the extractant of 40mL and 1g soil in step (1).
Embodiment 6
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the present embodiment and embodiment
4 unique difference are as follows: swirl mixing device oscillation 30s is uniformly dispersed after mixing the extractant of 10mL and 1g soil in step (1).
Comparative example 3
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the present embodiment and embodiment
4 unique difference are as follows: swirl mixing device oscillation 30s is uniformly dispersed after mixing the extractant of 5mL and 1g soil in step (1).
Embodiment 7
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the time that concussion is extracted in step (2) is 1h.
Embodiment 8
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the time that concussion is extracted in step (2) is 2h.
Embodiment 9
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the time that concussion is extracted in step (2) is 4h.
Embodiment 10
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the time that concussion is extracted in step (2) is 8h.
Embodiment 11
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the time that concussion is extracted in step (2) is 16h.
Embodiment 12
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the present embodiment and embodiment
4 unique difference are as follows: the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's
Concentration is 0.05mol/L, and the pH of mixed aqueous solution is 6.
Embodiment 13
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, the present embodiment and embodiment
1 unique difference are as follows: the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's
Concentration is 0.05mol/L, and the pH of mixed aqueous solution is 8.
Comparative example 4
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's
Concentration is 0.05mol/L, and the pH of mixed aqueous solution is 4.
Comparative example 5
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's
Concentration is 0.05mol/L, and the pH of mixed aqueous solution is 5.
Comparative example 6
As the extracting method of heavy metal available state in a kind of yellow moist soil of the embodiment of the present invention, this comparative example and embodiment
4 unique difference are as follows: the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2EDTA's
Concentration is 0.05mol/L, and the pH of mixed aqueous solution is 9.
Experimental example 1
GSF-2 yellow moist soil is applied to the extracting method of heavy metal available state in the moisture soil of embodiment 1-13, comparative example 1-6
(soil constituent analytical standard substance GBW07442) is quantified using ICP-MS after obtaining extracting solution, evaluates extracting method
Effect.
Content of beary metal/heavy metal in soil available state content (soil constituent analysis mark in recovery rate=extracting solution
Quasi- substance heavy metal available state asserting value)
Fig. 1 is the result figure of embodiment 1-3, comparative example 1-2, it was found that, Na2EDTA concentration is 0.05mol/L-
When 0.2mol/L, the content of heavy metal in soil available state is significantly higher, and overall cost considers, Na2EDTA concentration is
0.05mol/L is preferable.
Fig. 2 is the result figure of embodiment 4-6 and comparative example 3, it was found that, the amount ratio of the soil and extractant are as follows:
When 1:20g/mL-1:40g/mL, extraction efficiency is more preferable, comprehensively considers the recovery rate of three heavy metal species available states, soil and extraction
The amount ratio of agent are as follows: in comparison for recovery rate closer to 100%, effect is more preferable when 1:20g/mL.
Fig. 3 be embodiment 4, the result figure of embodiment 7-11, it was found that, shake extraction time be 0.5-1h when, mention
It takes effect preferable, and saves the time.
Fig. 4 is embodiment 4, the result figure of embodiment 12-13, comparative example 4-6, it was found that, when 4,5 pH, heavy metal
Zinc, arsenic recovery rate be more than 100%, show extractant pH be 4,5 when, there is the non-effective state heavy metal in part to be extracted to
In extracting solution, therefore, when evaluating the pollution risk of heavy metal in soil, the interference of non-effective state heavy metal will receive；It extracts
When the pH of agent is 6-7, both preferably avoided non-effective state landfill into extracting solution, moreover it is possible to keep a higher huge sum of money
Belong to the recovery rate of available state, effect is more preferable when evaluating the pollution risk of heavy metal in soil, and the pH compared to extractant is 7, mentions
Effect is more excellent when the pH of agent being taken to be 6.
The deviation using result of above-described embodiment and comparative example is less than 2%.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. the extracting method of heavy metal available state in a kind of yellow moist soil, which is characterized in that the described method comprises the following steps:
(1) extractant and soil are mixed and is uniformly dispersed, obtain extraction system；
Wherein, the extractant is Na2The mixed aqueous solution of EDTA and sodium hydroxide, Na in mixed aqueous solution2The concentration of EDTA is
0.05-0.2mol/L, the pH of mixed aqueous solution are 6-8；
(2) it is vortexed to extraction system or shakes extraction；
(3) it is separated by solid-liquid separation, collects extracting solution；
The wherein heavy metal are as follows: any combination of at least one of 3 heavy metal species of cadmium, zinc and arsenic heavy metal.
2. the method according to claim 1, wherein the pH of the mixed aqueous solution is 6-7.
3. method according to claim 1 or 2, which is characterized in that Na in the mixed aqueous solution2The concentration of EDTA is
0.05-0.1mol/L。
4. according to the method described in claim 3, it is characterized in that, the amount ratio of the soil and extractant are as follows: 1:10g/mL-
1:40g/mL。
5. according to the method described in claim 3, it is characterized in that, the amount ratio of the soil and extractant are as follows: 1:20g/mL.
6. according to the method described in claim 3, it is characterized in that, being in frequency of oscillation to extraction system in step (2)
200rpm horizontal oscillations shaking table extracts 0.5h or more.
7. according to the method described in claim 3, it is characterized in that, Na in the mixed aqueous solution2The concentration of EDTA is
0.05mol/L。
8. according to the method described in claim 3, it is characterized in that, the pH of the mixed aqueous solution is 6.
9. according to right want 1 described in method, which is characterized in that it is mixed by vortex after extractant and soil mixing in step (1)
Even device concussion is uniformly dispersed；Extraction system is kept to extract at 25 ± 2 DEG C in step (2).
10. the detection method of heavy metal available state in a kind of yellow moist soil, which is characterized in that the described method comprises the following steps:
(a) heavy metal available state in yellow moist soil is extracted by any the method for such as claim 1-9 and obtains extracting solution；
(b) it by extracting solution loading described in step (1), is quantified with ICP-MS.
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Application publication date: 20191018 |