CN102601107A - Solidifying processing method for estrogen compound in manganese dioxide doped soil - Google Patents
Solidifying processing method for estrogen compound in manganese dioxide doped soil Download PDFInfo
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- CN102601107A CN102601107A CN2012100543600A CN201210054360A CN102601107A CN 102601107 A CN102601107 A CN 102601107A CN 2012100543600 A CN2012100543600 A CN 2012100543600A CN 201210054360 A CN201210054360 A CN 201210054360A CN 102601107 A CN102601107 A CN 102601107A
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Abstract
The invention discloses a solidifying processing method for an estrogen compound in manganese dioxide doped soil and belongs to the technical field of solidifying processing for environmental pollutants. The solidifying processing method comprises the following steps of: adding manganese dioxide into soil and uniformly stirring so as to form a soil sample; taking and mixing a prepared estrogen compound aqueous solution with a certain amount of soil sample in a 100ml triangular flask; adjusting pH of soil water mixed solution to be within a range of 2.0-9.0; and performing adsorption reaction for 24 hours under an oscillating condition. The solidifying processing method provided by the invention has the advantages of simple operation, low cost, high removal rate of estrogen compound, excellent solidifying effect and the like; the removal rate of the estrogen compound in the aqueous solution is above 99%; the estrogen compound adsorbed into the soil sample is free from entering into the aqueous solution again under a desorption effect; and according to the method provided by the invention, the pollution of the estrogen compound in water body is efficiently reduced, the 'solidification' of the estrogen compound in soil is realized and the practicability and the application value are ultrahigh.
Description
Technical field
The invention belongs to fixedly processing technology field of environmental contaminants; Be particularly related to the immobilization processing method of estrogen compound in a kind of dopping manganese dioxide soil.
Technical background
Estrogen is through causing target cell to produce metabolism and physiological function that disorderly effect is disturbed organism with the incretory of organism, receptors bind on target cell; And then cause the internal system imbalance, destroy reproduction function and the normal metabolic of organism.Estrogen is again the major pollutants that the mankind and wildlife are feminized, even also can disturb the normal function of organism internal system when concentration is in ng/L.The pollution of estrogen compound is called as the third-largest global environmental problem after greenhouse gases, depletion of the ozone layer.Therefore, it is very necessary reducing estrogen compound research of animal migration in environment.
At present, control environment in the pollution migration of estrogen compound mainly concentrate on the correlative study that physisorphtion, chemical treatment advanced oxidation processes and biological degradation method etc. are removed estrogen compound in the water bodys.Sand, active carbon and resin material often are used as adsorbent the estrogen compound in the water body are adsorbed removal, and physisorphtion is simple to operate, but the estrogen compound after the absorption is prone to get into water body once more and causes secondary pollution.The scholar is arranged by TiO
2Technology such as light sensitivity, ultraviolet ray and ozone produce free radical (OH etc.) with strong oxidizing property; Through the free-radical oxidation degrading estrogen to reach the purpose that reduces the estrogen compound bio-toxicity; And the expensive of the technological practical application of this type, and water quality stability had relatively high expectations.Biologic treating technique has distinct advantages: 1. water environment is not produced secondary pollution, leftover problem is few; 2. in-situ treatment is easy and simple to handle, surrounding environment is disturbed few; 3. less reparation funds are merely the 30-50% that traditional chemical, physics are repaired funds; 4. the human chance that is directly exposed under these pollutants reduces.Yet also there are many shortcomings in biological degradation method, as: the biological degradation method microorganism used therefor needs prerequisite steps such as separation, purifying and cultivation, and the activated sludge that the biological treatment back produces still need carry out harmless treatment.Compare with biological degradation method with method of chemical treatment, physisorphtion is owing to simple to operate, cost and the short research focus that becomes of processing cycle.
Immobilization technology in the physisorphtion is a kind of in-situ treatment disposal technology, is regarded as potential effective pollutant in-situ treatment technology.Migration takes place and transforms and the entering surface water body in the estrogen compound in the soil under the effect of rainwashes such as rainfall; If suitably control external condition; Make the estrogen compound of labile state change stable state into, thereby then can significantly reduce the potential threat that probability that estrogen compound moves by soil reduces estrogen compound in water body.Through in soil, mix an amount of chemical reagent, mineral salt, organic matter etc., reduce the animal migration and the toxicity of pollutant, to realize the immobilization of estrogen compound in the soil.Documents and materials show; The research of immobilization technology biases toward the heavy metal pollution control in the soil more; As: adopt soil fixing heavy metal ion Pb, Cu, Cd and the Zn etc. of doped hydroxyapatite, and the immobilization research of estrogen compound does not appear in the newspapers in the relevant soil.
Summary of the invention
The purpose of this invention is to provide the immobilization processing method of estrogen compound in a kind of dopping manganese dioxide soil, it is characterized in that, the immobilization treatment step of said estrogen compound is following:
1) dopping manganese dioxide soil is to the immobilization of estrogen compound
(1) will be 1 by mass ratio: 200-30: 100 manganese dioxide and mixing with soil matter sample be put in the glass triangle bottle of 100mL, stir;
(2) with the pedotheque (g) of dopping manganese dioxide and the estrogen compound aqueous solution (mL) in 1: 400-1: 20 ratio; Add in the triangular flask; Regulate pH=2.0-9.0, under cyclotron oscillation device oscillating condition, carry out the adsorption experiment of the estrogen compound in the aqueous solution with 200r/min;
(3) persistent oscillation is 24 hours, behind the standing demix, adopts 0.45 μ m water system membrane filtration upper water solution, utilizes the amount of estrogen compound in the high-performance liquid chromatogram determination upper water solution;
2) mensuration of estrogen compound immobilization adsorbance
Dopping manganese dioxide soil adopts the immobilization adsorbance increase degree of estrogen compound to represent to the immobilization effect of estrogen compound; Adopt desorption method will not to be doped the estrogen compound wash-out of manganese dioxide soil fixingization; Utilize the soil that centrifugal method will adsorb estrogen compound to separate with the aqueous solution, then according to soil: secondary water=1: 400-1: the ratio of 20 (g/mL) is added secondary water in the triangular flask of 100mL, mixes mutually with soil behind the absorption estrogen compound; Regulate pH=2.0-9.0 identical when adsorbing; Regulating ionic strength with NaCl is 0.01mol/L, under the cyclotron oscillation device oscillating condition with 200r/min speed, carries out the estrogen compound that is not immobilized in the desorb soil; Vibration continues 24 hours; Behind the standing demix, adopt 0.45 μ m water system membrane filtration upper water solution, utilize the estrogen compound amount of desorb in the efficient liquid phase chromatographic analysis upper water solution; The immobilization adsorbance increase degree of estrogen compound is calculated as follows:
The immobilization adsorbance of D---estrogen compound increases degree, %;
Q
The contrast experiment---dopping manganese dioxide soil is not to the immobilization adsorbance of estrogen compound, mg/g.
3) effect experiment
(1) contrast experiment: take by weighing 0.7g and do not mix in the pedotheque 100mL glass triangle bottle; Is that 0.7: 40 (g/mL) pipettes the estrogen compound aqueous solution in pedotheque (g) in triangular flask with the estrogen compound aqueous solution (mL) ratio; Regulate pH=5.5; Under cyclotron oscillation device oscillating condition, carry out the estrogen compound in the adsorption aqueous solution with 200r/min speed.Vibration continues 24 hours; After the static layering; With 0.45 μ m water system membrane filtration upper water solution; Utilize high performance liquid chromatography quantitatively to filter the estrogen compound content in the upper water solution, utilize estrogen compound total amount in the aqueous solution to deduct the amount of estrogen compound in the upper solution then, calculate the adsorbance of estrogen compound
(2) immobilization experiment: get the 0.7g manganese dioxide that stirs and mixing with soil matter sample in 100mL glass triangle bottle; Pedotheque (g) in dopping manganese dioxide is that 0.7: 40 (g/mL) pipettes the estrogen compound aqueous solution in triangular flask with the estrogen compound aqueous solution (mL) ratio; Regulate pH=5.5; Under cyclotron oscillation device oscillating condition, carry out the estrogen compound in the adsorption aqueous solution with 200r/min speed.Vibration continues 24 hours; After the static layering; With 0.45 μ m water system membrane filtration upper water solution; Utilize high performance liquid chromatography quantitatively to filter the estrogen compound content in the upper water solution, utilize estrogen compound total amount in the aqueous solution to deduct the amount of estrogen compound in the upper solution then, calculate the adsorbance of estrogen compound
(3) soil of analyzing the pedotheque of dopping manganese dioxide and dopping manganese dioxide not respectively is to estrogenic adsorbance; Adopt above-mentioned formula contrast to know; In the soil behind the dopping manganese dioxide immobilization adsorbance of estrogen compound obviously increase; Experiment is compared through above-mentioned adsorption and desorption, is just to make estrogen compound immobilization more than 99% at 15% o'clock in soil at the doping ratio of manganese dioxide and soil, does not almost have estrogen compound to get into the aqueous solution once more owing to desorption; The clearance of estrogen compound is brought up to more than 99% in the aqueous solution; Explain that promptly manganese dioxide has strengthened estrogen compound stability in the soil, reduced the bioavailability of estrogen compound in the soil, reached the immobilization target of estrogen compound.
Said manganese dioxide is the above commercial reagent of chemical agent rank.
Described soil types is a yellowish soil.
Estrogen compound is natural estrogen (oestrone, estradiol, estriol) and artificial synthetic estrogen (17 α-ethinyl estradiol, bisphenol-A) a kind of individualism or multiple existence simultaneously in the said aqueous solution.
Good effect of the present invention: comparative analysis is known through the adsorption and desorption experimental result; The doping ratio of manganese dioxide and soil is just to make estrogen compound immobilization more than 99% at 15% o'clock in soil; Almost do not have estrogen compound to get into the aqueous solution once more owing to desorption, the clearance of estrogen compound is brought up to more than 99% in the aqueous solution; Manganese dioxide has strengthened the stability of estrogen compound in soil, has reduced the bioavailability of estrogen compound in the soil, has realized the immobilization of estrogen compound in the soil.
Use dopping manganese dioxide soil fixing estrogen compound of the present invention, simple to operate, expense is low, thereby have very high practicality and using value.
Description of drawings
Fig. 1 is the immobilization effect of embodiment 1 contrast experiment (not estrogen compound in the soil of dopping manganese dioxide).
The immobilization effect of Fig. 2 embodiment 2 immobilizations experiments 1 (estrogen compound in the soil of different manganese dioxide doped ratios).
The immobilization effect of Fig. 3 embodiment 3 immobilizations experiments 2 (estrogen compounds in the soil of different manganese dioxide doped ratios).
The specific embodiment
The present invention provides the immobilization processing method of estrogen compound in a kind of dopping manganese dioxide soil.The present invention uses the estrogen compound in the fixing absorption of the immobilization technology soil.Because estrogen compound comprises last over thousands of kinds such as natural estrogen, artificial synthetic, environmental contaminants and agricultural chemicals, therefore selects for use estrogen compound common in five kinds of soil (oestrone, estradiol, estriol, 17 α-ethinyl estradiol and bisphenol-A) to investigate the immobilization effect behind the dopping manganese dioxide in the soil as object.Characteristic of the present invention is the estrogen compound that utilizes in the adsorption by soil aqueous solution of dopping manganese dioxide; Centrifugation soil and water after absorption is accomplished; In solid phase, add 40mL secondary water then; The regulator solution ionic strength is 0.01mol/L, carries out desorption experiment under other condition condition identical with adsorption conditions, and wash-out is not doped the estrogen compound of manganese dioxide soil fixing.Obviously increase through the adsorbance of the soil behind the comparative analysis discovery dopping manganese dioxide estrogen compound; Increased substantially the clearance of estrogen compound in the aqueous solution; Also greatly reduce simultaneously the desorption quantity of estrogen compound, realized the immobilization of estrogen compound in the soil.Explain below in conjunction with accompanying drawing and embodiment.
Embodiment 1
The contrast experiment: take by weighing 0.7g yellowish soil as pedotheque in 100mL glass triangle bottle; Is that 0.7: 40 (g/mL) pipettes the estrogen compound aqueous solution in pedotheque (g) in triangular flask with the estrogen compound aqueous solution (mL) ratio; Regulate pH=5.5; Under cyclotron oscillation device oscillating condition, carry out the estrogen compound in the adsorption aqueous solution with 200r/min speed.Vibration continues 24 hours, after the static layering, with 0.45 μ m water system membrane filtration upper water solution.The concentration of upper water solution estrogen compound after upper water solution and the desorb after adopting efficient liquid phase chromatographic analysis to adsorb; Utilize estrogen compound total amount in the aqueous solution to deduct the amount of estrogen compound in the upper solution then; Calculate immobilization and be respectively 0.037mg/g (oestrone to the estrogen compound maximum in the soil; E1), 0.052mg/g (estradiol, E2), 0.064mg/g (17 α-ethinyl estradiol, EE2), 0.031mg/g (estriol; E3) and 0.031mg/g (bisphenol-A, BPA) (as shown in Figure 1).
Immobilization experiment 1: with mass ratio is that 1: 20 manganese dioxide and mixing with soil matter sample stirs; The manganese dioxide and the mixing with soil matter sample that take by weighing the 0.7g that stirs are in 100mL glass triangle bottle; Pedotheque (g) in dopping manganese dioxide is that 0.7: 40 (g/mL) pipettes the estrogen compound aqueous solution in triangular flask with the estrogen compound aqueous solution (mL) ratio; Regulate pH=5.5; Under cyclotron oscillation device oscillating condition, carry out the estrogen compound in the adsorption aqueous solution with 200r/min speed.Vibration continues 24 hours, after the static layering, with 0.45 μ m water system membrane filtration upper water solution.The concentration of upper water solution estrogen compound after upper water solution and the desorb after adopting efficient liquid phase chromatographic analysis to adsorb; Utilize estrogen compound total amount in the aqueous solution to deduct the amount of estrogen compound in the upper solution then, calculate the estrogen compound maximum that is adsorbed onto in the soil be respectively 0.17mg/g (oestrone, E1), 0.29mg/g (estradiol; E2), 0.26mg/g (17 α-ethinyl estradiol; EE2), 0.11mg/g (estriol, E3) and 0.15mg/g (bisphenol-A, BPA).(as shown in Figure 2).
Immobilization experiment 2: with mass ratio is that 3: 20 manganese dioxide and mixing with soil matter sample stirs; The manganese dioxide and the mixing with soil matter sample that take by weighing the 0.7g that stirs are in 100mL glass triangle bottle; Pedotheque (g) in dopping manganese dioxide is that 0.7: 40 (g/mL) pipettes the estrogen compound aqueous solution in triangular flask with the estrogen compound aqueous solution (mL) ratio; Regulate pH=5.5; Under cyclotron oscillation device oscillating condition, carry out the estrogen compound in the adsorption aqueous solution with 200r/min speed.Vibration continues 24 hours, after the static layering, with 0.45 μ m water system membrane filtration upper water solution.The concentration of upper water solution estrogen compound after upper water solution and the desorb after adopting efficient liquid phase chromatographic analysis to adsorb; Utilize estrogen compound total amount in the aqueous solution to deduct the amount of estrogen compound in the upper solution then, calculate the estrogen compound maximum that is adsorbed onto in the soil be respectively 1.89mg/g (estradiol, E2), 1.88mg/g (17 α-ethinyl estradiol; EE2), 1.32mg/g (estriol; E3) and 2.17mg/g (bisphenol-A, BPA), when oestrone concentration is lower than 1.2mg/L; Oestrone does not all detect in the upper water solution of absorption back, and oestrone all is immobilized.(as shown in Figure 3).
Claims (4)
1. the immobilization processing method of estrogen compound in the dopping manganese dioxide soil is characterized in that the immobilization treatment step of said estrogen compound is following:
1) dopping manganese dioxide soil is to the immobilization of estrogen compound
(1) will be 1 by mass ratio: 200-30: 100 manganese dioxide and mixing with soil matter sample be put in the glass triangle bottle of 100mL, stir;
(2) with the pedotheque (g) of dopping manganese dioxide and the estrogen compound aqueous solution (mL) in 1: 400-1: 20 ratio; Add in the triangular flask; Regulate pH=2.0-9.0, under cyclotron oscillation device oscillating condition, carry out the adsorption experiment of the estrogen compound in the aqueous solution with 200r/min;
(3) persistent oscillation is 24 hours, behind the standing demix, adopts 0.45 μ m water system membrane filtration upper water solution, utilizes the amount of estrogen compound in the high-performance liquid chromatogram determination upper water solution;
2) mensuration of estrogen compound immobilization adsorbance
Dopping manganese dioxide soil adopts the immobilization adsorbance increase degree of estrogen compound to represent to the immobilization effect of estrogen compound; Adopt desorption method will not to be doped the estrogen compound wash-out of manganese dioxide soil fixingization; Utilize the soil that centrifugal method will adsorb estrogen compound to separate with the aqueous solution, then according to soil: secondary water=1: 400-1: the ratio of 20 (g/mL) is added secondary water in the triangular flask of 100mL, mixes mutually with soil behind the absorption estrogen compound; Regulate pH=2.0-9.0 identical when adsorbing; Regulating ionic strength with NaCl is 0.01mol/L, under the cyclotron oscillation device oscillating condition with 200r/min speed, carries out the estrogen compound that is not immobilized in the desorb soil; Vibration continues 24 hours; Behind the standing demix, adopt 0.45 μ m water system membrane filtration upper water solution, utilize the estrogen compound amount of desorb in the efficient liquid phase chromatographic analysis upper water solution; The immobilization adsorbance increase degree of estrogen compound is calculated as follows:
The immobilization adsorbance of D---estrogen compound increases degree, %;
Q
The contrast experiment---dopping manganese dioxide soil is not to the immobilization adsorbance of estrogen compound, mg/g.
3) effect experiment
(1) contrast experiment: take by weighing 0.7g and do not mix pedotheque in 100mL glass triangle bottle; Is that 0.7: 40 (g/mL) pipettes the estrogen compound aqueous solution in pedotheque (g) in triangular flask with the estrogen compound aqueous solution (mL) ratio; Regulate pH=5.5; Under cyclotron oscillation device oscillating condition, carry out the estrogen compound in the adsorption aqueous solution with 200r/min speed.Vibration continues 24 hours, after the static layering, with 0.45 μ m water system membrane filtration upper water solution, utilizes high performance liquid chromatography quantitative; Utilize estrogen compound total amount in the aqueous solution to deduct the amount of estrogen compound in the upper solution then, calculate the adsorbance of estrogen compound;
(2) immobilization experiment: get the 0.7g manganese dioxide that stirs and mixing with soil matter sample in 100mL glass triangle bottle; Pedotheque (g) in dopping manganese dioxide is that 0.7: 40 (g/mL) pipettes the estrogen compound aqueous solution in triangular flask with the estrogen compound aqueous solution (mL) ratio; Regulate pH=5.5; Under cyclotron oscillation device oscillating condition, carry out the estrogen compound in the adsorption aqueous solution with 200r/min speed.Vibration continues 24 hours; After the static layering; With 0.45 μ m water system membrane filtration upper water solution, utilize high performance liquid chromatography quantitatively to utilize estrogen compound total amount in the aqueous solution to deduct the amount of estrogen compound in the upper solution then, calculate the adsorbance of estrogen compound;
(3) soil of analyzing the pedotheque of dopping manganese dioxide and dopping manganese dioxide not respectively is to estrogenic adsorbance; Adopt above-mentioned formula contrast to know; In the soil behind the dopping manganese dioxide immobilization adsorbance of estrogen compound obviously increase; Experiment is compared through above-mentioned adsorption and desorption, is just to make estrogen compound immobilization more than 99% at 15% o'clock in soil at the doping ratio of manganese dioxide and soil, does not almost have estrogen compound to get into the aqueous solution once more owing to desorption; The clearance of estrogen compound is brought up to more than 99% in the aqueous solution; Explain that promptly manganese dioxide has strengthened estrogen compound stability in the soil, reduced the bioavailability of estrogen compound in the soil, reached the immobilization target of estrogen compound.
2. according to the immobilization processing method of estrogen compound in the said dopping manganese dioxide soil of claim 1, it is characterized in that said manganese dioxide is the above commercial reagent of chemical agent rank.
3. according to the immobilization processing method of estrogen compound in the said dopping manganese dioxide soil of claim 1, it is characterized in that described soil types is a yellowish soil.
4. according to the immobilization processing method of estrogen compound in the said dopping manganese dioxide soil of claim 1, it is characterized in that estrogen compound is a natural estrogen in the said aqueous solution: oestrone, estradiol and estriol; Exist simultaneously with one or more of individualism in artificial synthetic estrogen: 17 α-ethinyl estradiol and the bisphenol-A.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112023983A (en) * | 2020-08-31 | 2020-12-04 | 安徽工业大学 | Ozone catalyst for environmental estrogen and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003080225A (en) * | 2001-09-12 | 2003-03-18 | Sekisui Chem Co Ltd | Soil cleaning method by cyclodextrins immobilizing adsorbent |
| EP1857541A1 (en) * | 2005-02-23 | 2007-11-21 | Kabushiki Kaisha Yakult Honsha | Estrogenic substance degradable microorganism and use thereof |
| CN101306864A (en) * | 2008-06-25 | 2008-11-19 | 浙江工业大学 | Degradation process for environment estrogenic pollutant in water body |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003080225A (en) * | 2001-09-12 | 2003-03-18 | Sekisui Chem Co Ltd | Soil cleaning method by cyclodextrins immobilizing adsorbent |
| EP1857541A1 (en) * | 2005-02-23 | 2007-11-21 | Kabushiki Kaisha Yakult Honsha | Estrogenic substance degradable microorganism and use thereof |
| CN101306864A (en) * | 2008-06-25 | 2008-11-19 | 浙江工业大学 | Degradation process for environment estrogenic pollutant in water body |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112023983A (en) * | 2020-08-31 | 2020-12-04 | 安徽工业大学 | Ozone catalyst for environmental estrogen and preparation method and application thereof |
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Application publication date: 20120725 |