CN109959727A - A kind of application of chemical reagent formulation in detection heavy metal pollution of soil - Google Patents
A kind of application of chemical reagent formulation in detection heavy metal pollution of soil Download PDFInfo
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- CN109959727A CN109959727A CN201711424666.XA CN201711424666A CN109959727A CN 109959727 A CN109959727 A CN 109959727A CN 201711424666 A CN201711424666 A CN 201711424666A CN 109959727 A CN109959727 A CN 109959727A
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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
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Abstract
A kind of application of the chemical reagent formulation of the present invention in detection heavy metal pollution of soil, first pass through soil sample, alkaline hydrolysis, acid mentions, is concentrated, micro-filtration and constant volume, blank solution and quantitative determination are prepared again, the present invention is sensitiveer in detection heavy metal in soil content, detection efficiency with higher, have many advantages, such as the rate of recovery is good, precision is high, processing speed is fast, it is easy to operate, be applicable in wide model.
Description
Technical field
The present invention relates to soil pollution processing technology fields, and in particular to a kind of chemical reagent formulation is in a detection soil huge sum of money
Belong to the application in pollution.
Background technique
Soil pollution is since the harmful substance contained in soil is excessive, has been more than the self-purification capacity of soil, so as to cause
Composition of the soil, structure and function change, and harmful substance is built up in the soil, pass through " soil → plant → people
Body ", or be absorbed by the body indirectly by " soil → water → human body ", reach the degree being detrimental to health.Heavy metal-polluted soil is dirty
Dye mainly includes the significant elements of bio-toxicities such as mercury (Hg), cadmium (Cd), lead (Pb), chromium (Cr) and metalloid arsenic (As), and
Have an elements such as the zinc (Zn), copper (Cu), nickel (Ni) of certain toxicity, vertical distribution in the soil poor mobility, when being detained
Between transformation and migration long, that form can only occur, cannot be degraded by microorganisms." Itai-itai diseases " and " minamata disease " occurred in history
Precisely due to heavy metal pollution and pathogenic typical case.Therefore, the effective restorative procedure for exploring heavy metal pollution of soil becomes
The task of top priority.
Currently, the method that the traditional improvement restorative procedure of heavy metal pollution of soil is usually physics and chemistry, such as dilution and
Covering method, vitrification, heat treatment technics, elution method, electrochemical process etc., traditional restorative procedure is at high cost, it is lasting to repair
Time length, slow effect, heavy metal contaminants generally form complex compound, are only the harm for reducing heavy metal, can not be by heavy metal
It is removed from soil, easily causes the secondary pollution of soil.
Summary of the invention
(1) technical problems to be solved
In order to overcome the shortage of prior art, it is proposed that a kind of application of chemical reagent formulation in detection heavy metal pollution of soil,
To solve the problems mentioned in the above background technology.
(2) technical solution
Of the invention is achieved through the following technical solutions: a kind of chemical reagent formulation answering in detection heavy metal pollution of soil
With, comprising the following steps:
One, the sample pretreatment stage
1) alkaline hydrolysis: precision weighs pedotheque 5g, and the dilute alkaline soln that 10mL contains ammonium chloride is added, after shaking through microwave at
Reason, obtains alkaline hydrolysis sample solution,
2) acid mentions: acid mentions: 20mL being contained to the dilute acid soln of hydrogen peroxide, is quickly adding into step 1 institute under agitation
Alkaline hydrolysis sample solution in, detect pH value of solution, pH value if more than 2, adjust pH value to less than or after being equal to 2, surpassed
Sound extracts, and centrifugation, residue is washed with the dilute acid soln containing hydrogen peroxide, is centrifuged, and merges supernatant, obtains crude extract；It is described
Dilute acid soln containing hydrogen peroxide is prepared before use,
3) it is concentrated: crude extract is concentrated, concentrate is made,
4) micro-filtration: by concentrate with being filtered, being made refined filtration liquid,
5) constant volume: refined filtration liquid acid solution is diluted into simultaneously constant volume, refined filtration liquid is made:
Two, the quantitative measurment stage
1) it prepares blank solution: measuring the dilute alkaline soln that 10mL contains ammonium chloride, after microwave treatment, under agitation rapidly
It 20mL is added and contains the dilute acid soln of hydrogen peroxide, is ultrasonically treated, is centrifuged, residue is with described containing hydrogen peroxide
Dilute acid soln washing, centrifugation, merge supernatant after, through rotary evaporating device concentration, then filter, last constant volume to get
Blank solution,
2) it quantitative determines: test solution obtained by step 5 being quantitative determined using using atomic absorption spectrophotometry,
Atomic absorption spectrophotometry is respectively: the measurement of lead uses graphite furnace-atomic absorption, and Cadmium detrmination uses stone
Black furnace-atomic absorption, the measurement of arsenic use hydride generation-atomic absorption, and Cupper determination is using fire
Flame-atomic absorption.
Furthermore, the aqueous slkali is the mixture of sodium hydroxide and potassium hydroxide, the concentration of hydroxide ion
For 0,5-1 .5mol/L, the mass fraction of the ammonium hydroxide is 8- 12%.
Furthermore, the aqueous slkali is the mixture of sodium hydroxide and potassium hydroxide, the concentration of hydroxide ion
For 0,8mol/L, the mass fraction of the ammonium hydroxide is 10%.
Furthermore, the acid solution is the mixture of sulfuric acid solution, hydrochloric acid solution, citric acid solution, hydrionic
Concentration is greater than or equal to 0,2-0 .5mol/L；The hypochlorous mass fraction is 4-6%.
Furthermore, the acid solution is the mixture of sulfuric acid solution, hydrochloric acid solution, citric acid solution, hydrionic
Concentration is greater than or equal to 0,3mol/L；The hypochlorous mass fraction is 5%.
Furthermore, the miillpore filter is PVDF material.
Furthermore, the chromatographic column is ACQUITYUPLC BEH C18, and chromatographic column specification is 1 .7 μm, 2 .1 ×
50mm, mobile phase are water-methanol gradient elution, and the time is respectively 0,1 .1,2,3,4,7,8,8 .5, water and first at 11 minutes
The mass percent of alcohol is respectively 100:0,100:0,98:2,90:10,85:15,0:100,0:100,100:0,100:0, inspection
Survey wavelength 254nm, flow velocity 0.5mLmin-1,5 μ l of sample volume, with external standard method with calculated by peak area.
(3) beneficial effect
The present invention compared with the existing technology, has the advantages that
Application of a kind of chemical reagent formulation that the present invention mentions in detection heavy metal pollution of soil, using alkaline hydrolysis acid formulation
Sample is pre-processed, the loss and air pollution of heavy metal element are avoided；Concentration step is increased, to heavy metal member
The low-down sample of element after can increasing sample weighting amount, carries out concentration to crude extract, to improve a huge sum of money in test solution
The concentration of category, to increase the sensitivity of sample measurement.Sample of the present invention after pretreatment, can be used for detection device for multi metallic elements
Measurement, do not need the pretreatment that every Heavy Metallic Elements individually carry out sample, reduce workload.The present invention is in detection soil
It is sensitiveer on content of beary metal in earth, detection efficiency with higher, have the rate of recovery is good, precision is high, processing speed is fast,
It is easy to operate, be applicable in the advantages that wide model.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, it should be understood that tool described herein
Body embodiment is only used to explain the present invention, is not intended to limit the present invention.
A kind of specific embodiment 1: the application of chemical reagent formulation in detection heavy metal pollution of soil, it is characterised in that:
The following steps are included:
One, the sample pretreatment stage
1) alkaline hydrolysis: weighing soil 3g, and the aqueous slkali that 8mL contains ammonium hydroxide is added, in the item that power is 0 .6 kw of power after shaking
Microwave treatment 40 seconds under part, obtain alkaline hydrolysis sample solution；The aqueous slkali is the mixture of sodium hydroxide and potassium hydroxide, hydrogen-oxygen
The concentration of radical ion is 0,5mol/L, and the mass fraction of the ammonium hydroxide is 8%.
2) acid mentions: 18mL being contained hypochlorous acid solution, is quickly adding into the resulting alkali of step 1) under agitation
It solves in sample solution, detects pH value of solution, and adjust pH value to after 2, carry out ultrasound under conditions of 25 DEG C of temperature, 250W, 40kHz and mention
20min is taken, is centrifuged, residue, which is used, contains hypochlorous acid solution wash, and centrifugation merges supernatant, and crude extract is made.The acid is molten
Liquid is the mixture of sulfuric acid solution, hydrochloric acid solution, citric acid solution, and hydrionic concentration is greater than or equal to 0,2mol/L；Institute
Stating hypochlorous mass fraction is 4%.
3) it is concentrated: crude extract being concentrated using rotary evaporating device, concentrate is made.
4) by 0 .2 μm of filtering with microporous membrane of concentrate, refined filtration liquid micro-filtration: is made.Miillpore filter is PVDF material.
5) constant volume: refined filtration liquid acid solution is diluted into simultaneously constant volume, test solution is made.
Two, the quantitative measurment stage
1) it prepares blank solution: measuring the aqueous slkali that 8mL contains ammonium hydroxide, after microwave treatment, be rapidly added under agitation
18mL contains hypochlorous acid solution, detects pH value of solution, adjusts pH value to after 2, under conditions of 25 DEG C of temperature, 250W, 40kHz into
Row ultrasonic extraction 20min, centrifugation, the residue hypochlorous acid solution wash that contains, centrifugation, after merging supernatant, warp
Rotary evaporating device concentration, then with 0 .2 μm of filtering with microporous membrane, last constant volume is to get blank solution.
2) it quantitative determines: gained test solution being quantitative determined using ultra-performance liquid chromatography.Color used
Spectrum column is ACQUITYUPLC BEH C18, and chromatographic column specification is 1 .7 μm, 2 .1 × 50mm, and mobile phase is that water-methanol gradient is washed
De-, the time is respectively 0,1 .1,2,3,4,7,8,8 .5, and the mass percent of water and methanol is respectively 100:0 at 11 minutes,
100:0,98:2,90:10,85:15,0:100,0:100,100:0,100:0, Detection wavelength 254nm, 0 .5mL of flow velocity
Min-1,5 μ L of sample volume, with external standard method with calculated by peak area
A kind of specific embodiment 2: the application of chemical reagent formulation in detection heavy metal pollution of soil, it is characterised in that: including
Following steps:
One, the sample pretreatment stage
1) alkaline hydrolysis: weighing soil 8g, and the aqueous slkali that 12mL contains ammonium hydroxide is added, in the item that power is 0 .8 kw of power after shaking
Microwave treatment 80 seconds under part, obtain alkaline hydrolysis sample solution；The aqueous slkali is the mixture of sodium hydroxide and potassium hydroxide, hydroxyl
The concentration of ion is 1 .5mol/L, and the mass fraction of the ammonium hydroxide is 12%.
2) acid mentions: 22mL being contained hypochlorous acid solution, is quickly adding into the resulting alkali of step 1) under agitation
It solves in sample solution, detects pH value of solution, and adjust pH value to after 5, carry out ultrasound under conditions of 35 DEG C of temperature, 350W, 50kHz and mention
30min is taken, is centrifuged, residue, which is used, contains hypochlorous acid solution wash, and centrifugation merges supernatant, and crude extract is made.The acid is molten
Liquid is the mixture of sulfuric acid solution, hydrochloric acid solution, citric acid solution, and hydrionic concentration is greater than or equal to 0 .5mol/L；It is described
Hypochlorous mass fraction is 6%.
3) it is concentrated: crude extract being concentrated using rotary evaporating device, concentrate is made.
4) by 0 .8 μm of filtering with microporous membrane of concentrate, refined filtration liquid micro-filtration: is made.Miillpore filter is PVDF material.
5) constant volume: refined filtration liquid acid solution is diluted into simultaneously constant volume, test solution is made.
Two, the quantitative measurment stage
1) it prepares blank solution: measuring the aqueous slkali that 12mL contains ammonium hydroxide, after microwave treatment, be rapidly added under agitation
18-22mL contains hypochlorous acid solution, detects pH value of solution, adjusts pH value to after 5, in 35 DEG C of temperature, the condition of 350W, 50kHz
Lower progress ultrasonic extraction 30min, centrifugation, residue merge supernatant with the hypochlorous acid solution wash that contains, centrifugation
Afterwards, through rotary evaporating device concentration, then with 0 .8 μm of filtering with microporous membrane, last constant volume is to get blank solution.
2) it quantitative determines: gained test solution being quantitative determined using ultra-performance liquid chromatography.Color used
Spectrum column is ACQUITYUPLC BEH C18, and chromatographic column specification is 1 .7 μm, 2 .1 × 50mm, and mobile phase is that water-methanol gradient is washed
De-, the time is respectively 0,1 .1,2,3,4,7,8,8 .5, and the mass percent of water and methanol is respectively 100:0 at 11 minutes,
100:0,98:2,90:10,85:15,0:100,0:100,100:0,100:0, Detection wavelength 254nm, 0 .5mL of flow velocity
Min-1,5 μ L of sample volume, with external standard method with calculated by peak area.
A kind of specific embodiment 3: the application of chemical reagent formulation in detection heavy metal pollution of soil, it is characterised in that:
The following steps are included:
One, the sample pretreatment stage
1) alkaline hydrolysis: weighing soil 5g, and the aqueous slkali that 10mL contains ammonium hydroxide is added, in the item that power is 0 .7 kw of power after shaking
Microwave treatment 60 seconds under part, obtain alkaline hydrolysis sample solution；The aqueous slkali is the mixture of sodium hydroxide and potassium hydroxide, hydroxyl
The concentration of ion is 0 .8mol/L, and the mass fraction of the ammonium hydroxide is 10%.
2) acid mentions: 20mL being contained hypochlorous acid solution, is quickly adding into the resulting alkali of step 1) under agitation
It solves in sample solution, detects pH value of solution, and adjust pH value to after 4, surpassed under conditions of 30 DEG C of temperature, 300W, 40-50kHz
Sound extracts 20-30min, centrifugation, and residue, which is used, contains hypochlorous acid solution wash, and centrifugation merges supernatant, and crude extract is made.
The acid solution is the mixture of sulfuric acid solution, hydrochloric acid solution, citric acid solution, and hydrionic concentration is greater than or equal to 0,
3mol/L；The hypochlorous mass fraction is 5%.
3) it is concentrated: crude extract being concentrated using rotary evaporating device, concentrate is made.
4) by the concentrate filtering with microporous membrane of 0 .2-0 .8 μm, refined filtration liquid micro-filtration: is made.Miillpore filter is PVDF
Material.
5) constant volume: refined filtration liquid acid solution is diluted into simultaneously constant volume, test solution is made.
Two, the quantitative measurment stage
1) it prepares blank solution: measuring the aqueous slkali that 8-12mL contains ammonium hydroxide, after microwave treatment, be rapidly added under agitation
18-22mL contains hypochlorous acid solution, detects pH value of solution, after adjusting pH value to 2-5, in 25-35 DEG C of temperature, 250-350W, 40-
Ultrasonic extraction 20-30min, centrifugation are carried out under conditions of 50kHz, residue contains hypochlorous acid solution wash with described, from
The heart, it is finally fixed then with the filtering with microporous membrane of 0 .2-0 .8 μm through rotary evaporating device concentration after merging supernatant
Hold to get blank solution.
2) it quantitative determines: gained test solution being quantitative determined using ultra-performance liquid chromatography.Color used
Spectrum column is ACQUITYUPLC BEH C18, and chromatographic column specification is 1 .7 μm, 2 .1 × 50mm, and mobile phase is that water-methanol gradient is washed
De-, the time is respectively 0,1 .1,2,3,4,7,8,8 .5, and the mass percent of water and methanol is respectively 100:0 at 11 minutes,
100:0,98:2,90:10,85:15,0:100,0:100,100:0,100:0, Detection wavelength 254nm, 0 .5mL of flow velocity
Min-1,5 μ L of sample volume, with external standard method with calculated by peak area.
A kind of application of the chemical reagent formulation that the present invention mentions in detection heavy metal pollution of soil, is mentioned using alkaline hydrolysis acid
Method pre-processes sample, avoids the loss and air pollution of heavy metal element；Concentration step is increased, to heavy metal
The low-down sample of element after can increasing sample weighting amount, carries out concentration to crude extract, to improve weight in test solution
The concentration of metal, to increase the sensitivity of sample measurement.Sample of the present invention after pretreatment, can be used for various heavy
The measurement of element does not need the pretreatment that every Heavy Metallic Elements individually carry out sample, reduces workload.The present invention is examining
Sensitiveer, detection efficiency with higher in heavy metal in soil content is surveyed, with the rate of recovery is good, precision is high, processing is fast
Spend it is fast, easy to operate, be applicable in the advantages that wide model.
The above-described embodiments are merely illustrative of preferred embodiments of the present invention, not to structure of the invention
Think and range is defined.Without departing from the design concept of the invention, ordinary people in the field is to technology of the invention
The all variations and modifications that scheme is made, should all drop into protection scope of the present invention, the claimed technology contents of the present invention,
It is all described in the claims.
Claims (5)
1. a kind of application of chemical reagent formulation in detection heavy metal pollution of soil, it is characterised in that: the following steps are included:
One, the sample pretreatment stage
1) alkaline hydrolysis: precision weighs pedotheque 5g, and the dilute alkaline soln that 10mL contains ammonium chloride is added, after shaking through microwave at
Reason, obtains alkaline hydrolysis sample solution,
2) acid mentions: 20mL being contained to the dilute acid soln of hydrogen peroxide, it is resulting to be quickly adding into step 1 under agitation
In alkaline hydrolysis sample solution, detect pH value of solution, pH value if more than 2, adjust pH value to less than or after being equal to 2, carry out ultrasound and mention
It takes, is centrifuged, residue is washed with the dilute acid soln containing hydrogen peroxide, is centrifuged, and is merged supernatant, is obtained crude extract；It is described to contain mistake
The dilute acid soln of hydrogen oxide is prepared before use,
3) it is concentrated: crude extract is concentrated, concentrate is made,
4) micro-filtration: by concentrate with being filtered, being made refined filtration liquid,
5) constant volume: refined filtration liquid acid solution is diluted into simultaneously constant volume, refined filtration liquid is made:
Two, the quantitative measurment stage
1) blank solution is prepared:: measure the 10mL dilute alkaline soln that contains ammonium chloride, after microwave treatment, under agitation rapidly
It 20mL is added and contains the dilute acid soln of hydrogen peroxide, is ultrasonically treated, is centrifuged, residue is with described containing hydrogen peroxide
Dilute acid soln washing, centrifugation, merge supernatant after, through rotary evaporating device concentration, then filter, last constant volume to get
Blank solution,
2) it quantitative determines: test solution obtained by step 5 being quantitative determined using using atomic absorption spectrophotometry,
Atomic absorption spectrophotometry is respectively: the measurement of lead uses graphite furnace-atomic absorption, and Cadmium detrmination uses stone
Black furnace-atomic absorption, the measurement of arsenic use hydride generation-atomic absorption, and Cupper determination is using fire
Flame-atomic absorption.
2. a kind of application of the chemical reagent formulation according to claim 1 in detection heavy metal pollution of soil, feature
Be: it is described state dilute alkaline soln be one or both of sodium hydroxide solution, potassium hydroxide solution, concentration be 0.2~
1.0mol/L, the concentration of the ammonium chloride are mass fraction 10%.
3. a kind of application of the chemical reagent formulation according to claim 1 in detection heavy metal pollution of soil, feature
Be: the acid solution is the mixture of sulfuric acid solution, hydrochloric acid solution, citric acid solution, and hydrionic concentration is greater than or equal to 0
. 2-0 .5mol/L；The hypochlorous mass fraction is 4-6%.
4. a kind of application of the chemical reagent formulation according to claim 1 in detection heavy metal pollution of soil, feature
Be: the acid solution is the mixture of sulfuric acid solution, hydrochloric acid solution, citric acid solution, and hydrionic concentration is greater than or equal to
0 . 3mol/L；The hypochlorous mass fraction is 5%.
5. a kind of application of the chemical reagent formulation according to claim 1 in detection heavy metal pollution of soil, feature
Be: the dilute alkaline soln is sodium hydroxide solution, and the concentration of sodium hydroxide solution is 0.5mol/L, and microwave power is
800W, microwave time are 30s, and dilute acid soln described in step 2 is hydrochloric acid solution, and the concentration of hydrochloric acid solution is 0.5mol/L,
The ultrasonic extraction time is 20min.
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| CN201711424666.XA CN109959727A (en) | 2017-12-26 | 2017-12-26 | A kind of application of chemical reagent formulation in detection heavy metal pollution of soil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN114755352A (en) * | 2022-03-25 | 2022-07-15 | 煤炭科学技术研究院有限公司 | Method for measuring content of heavy metal elements in garbage and application |
-
2017
- 2017-12-26 CN CN201711424666.XA patent/CN109959727A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN111442960B (en) * | 2020-04-20 | 2023-12-29 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN114755352A (en) * | 2022-03-25 | 2022-07-15 | 煤炭科学技术研究院有限公司 | Method for measuring content of heavy metal elements in garbage and application |
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Application publication date: 20190702 |