CN103439430A - Method for determining bioavailability polycyclic aromatic hydrocarbon content in soil based on thermal desorption treatment - Google Patents
Method for determining bioavailability polycyclic aromatic hydrocarbon content in soil based on thermal desorption treatment Download PDFInfo
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- CN103439430A CN103439430A CN2013103862176A CN201310386217A CN103439430A CN 103439430 A CN103439430 A CN 103439430A CN 2013103862176 A CN2013103862176 A CN 2013103862176A CN 201310386217 A CN201310386217 A CN 201310386217A CN 103439430 A CN103439430 A CN 103439430A
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Abstract
The invention discloses a method for determining bioavailability polycyclic aromatic hydrocarbon content in soil based on thermal desorption treatment. The method specifically comprises the following steps: dividing a soil sample to be determined into two parts, determining the polycyclic aromatic hydrocarbon content in one part before treatment by adopting an acetone solvent extraction method, carrying out thermal desorption treatment on the other part to remove bioavailability polycyclic aromatic hydrocarbon in the sample firstly and then determining the polycyclic aromatic hydrocarbon content after treatment by adopting the acetone solvent extraction method, so that a difference value between the polycyclic aromatic hydrocarbon content before the treatment and the polycyclic aromatic hydrocarbon content after the treatment is the bioavailability polycyclic aromatic hydrocarbon content in the soil sample. The method has the advantages that thermal desorption treatment time is short, a quick and convenient method for determining the bioavailability polycyclic aromatic hydrocarbon content in the soil is provided, the determination time of the bioavailability polycyclic aromatic hydrocarbon content in the soil is greatly shortened, and the method is easy and convenient to operate, low in cost and good in repeatability, and has good popularization significance.
Description
Technical field
The present invention relates to the soil pollutant technical field of analysis and detection, relate in particular to a kind of method of measuring biologically effective state polycyclic aromatic hydrocarbon content in soil of processing based on thermal desorption.
Background technology
Change aromatic hydrocarbons (PAHs) is the Typical Organic Pollutants that a class is very paid close attention in the world more, has teratogenesis, carcinogenic and mutagenicity, wherein has 16 kinds of components by Environmental Protection Agency, to be listed in preferential control list.
Palycyclic aromatic in soil can be divided into can extract state and residual form.Can extract that in state, some is easy to be utilized by biology, be called the biologically effective state, remainder is difficult to by biological utilisation.
Estimate the biologically effective state content of PAHs in soil, method commonly used comprises biological method and chemical method.Biological method can directly be assessed toxicity and the biological effectiveness of PAHs in soil, tool intuitive, and its shortcoming is time-consuming longer, expense is too high.HP-β-CD (HPCD) extraction, accelerated solvent extraction (the Accelerated Solvent Extraction of comprising commonly used in physico-chemical process, ASE), supercritical fluid extraction (Supercritical Fluid Extraction, SFE), resin extraction etc.ASE and SFE are consuming time shorter, but the equipment needed thereby price is higher, as the routine monitoring method, certain difficulty are arranged.It is longer that HPCD and resin extract spent time, and the former needs tens hours, and the latter does not wait to January in one week consuming time.Cuypers proposes to adopt potassium persulfate oxidation method can comparatively fast remove biologically effective state palycyclic aromatic in soil, provide pre-treating method preferably for shortening minute, but this pretreatment process needs 3h, and the time is still longer, and complex operation.Therefore, set up a kind of assay method shorter, easy and simple to handle, biologically effective state palycyclic aromatic that expense is lower consuming time and seem particularly necessary.
Summary of the invention
The method that the purpose of this invention is to provide biologically effective state polycyclic aromatic hydrocarbon content in a kind of short, easy and simple to handle, mensuration soil that expense is lower consuming time.
Processing based on thermal desorption the method for measuring biologically effective state polycyclic aromatic hydrocarbon content in soil in the present invention mainly comprises the following steps:
1, pedotheque preparation: by the pedotheque natural air drying, the soil after air-dry grinds and crosses 20 mesh sieves, and collecting sieves sieves for next step;
2, methylene chloride and acetone hybrid extraction liquid polycyclic aromatic hydrocarbon content mensuration before the processing: get 3g drying and screening pedotheque, add the 1:1(volume ratio of 10mL), ultrasonic extraction 10 minutes, centrifugal, collect supernatant, again add extract, repeat 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured.
3, thermal desorption is processed: get 100g drying and screening pedotheque, soil sample is put into to Soil Thermal desorption rotary furnace (Soil Thermal desorption rotary furnace test macro, the patent No.: ZL 2,012 2 0468562.5) Quartz stove tube in, with the stove hook, soil sample is shifted onto to the constant temperature zone position of Quartz stove tube middle, then install flange, open carrier gas, regulate Soil Thermal desorption rotary furnace test macro, be 20-40min heat time heating time, preferably 30min, heating-up temperature is 150-300 ℃, preferably 200-250 ℃.After heating finishes, continue logical carrier gas cooling to soil sample, then close carrier gas, the outlet side of unloading the pipe type rotary furnace is connected with the flange of the air pressure valve of giving vent to anger, adjust the Quartz stove tube inclination angle, make soil sample from landing in Quartz stove tube, by soil sample collection (Soil Thermal desorption rotary furnace test macro and method of testing thereof, application number: 201210340236.0).
4, methylene chloride and acetone hybrid extraction liquid polycyclic aromatic hydrocarbon content mensuration after the thermal desorption processing: get 3g and process rear pedotheque, add the 1:1(volume ratio of 10mL), ultrasonic extraction 10 minutes, centrifugal, the collection supernatant, add extract again, repeats 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured.
5, biologically effective state polycyclic aromatic hydrocarbon content calculates: polycyclic aromatic hydrocarbon content after polycyclic aromatic hydrocarbon content before biologically effective state polycyclic aromatic hydrocarbon content=processing-processing.
The invention has the advantages that:
Thermal desorption is processed consuming time shorter, and with respect to other method of testings, its operation is more easy, provide pre-treating method quickly and easily for measuring biological effectiveness polycyclic aromatic hydrocarbon content in soil, greatly shortened the time that in soil, biologically effective state polycyclic aromatic hydrocarbon content is measured, in addition, the thermal desorption disposal cost is lower, reproducible, there is dissemination preferably.
Embodiment
The following examples are to describe in further detail of the present invention.
Embodiment 1:
1, the preparation of pedotheque: sample collection is from certain coke-oven plant's Polluted Soil, and polycyclic aromatic hydrocarbon content is lower.The pedotheque natural air drying that to gather, the soil after air-dry grinds and crosses 20 mesh sieves, and collecting sieves sieves for next step.
2, methylene chloride and acetone hybrid extraction liquid Polycyclic aromatic hydrocarbons assay before the processing: get 3g drying and screening pedotheque, add the 1:1(volume ratio of 10mL), ultrasonic extraction 10 minutes, centrifugal, collect supernatant, again add extract, repeat 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured, and result is 432.4mg/kg.
3, thermal desorption is processed: get 100g drying and screening pedotheque, soil sample is put into to Soil Thermal desorption rotary furnace (Soil Thermal desorption rotary furnace test macro, the patent No.: ZL 2,012 2 0468562.5) Quartz stove tube in, with the stove hook, soil sample is shifted onto to the constant temperature zone position of Quartz stove tube middle, then install flange, open carrier gas, regulate Soil Thermal desorption rotary furnace test macro, be 30min heat time heating time, and heating-up temperature is 220 ℃.After heating finishes, continue logical carrier gas cooling to soil sample, then close carrier gas, the outlet side of unloading the pipe type rotary furnace is connected with the flange of the air pressure valve of giving vent to anger, adjust the Quartz stove tube inclination angle, make soil sample from landing in Quartz stove tube, by soil sample collection (Soil Thermal desorption rotary furnace test macro and method of testing thereof, application number: 201210340236.0).
4, methylene chloride and acetone hybrid extraction liquid polycyclic aromatic hydrocarbon content mensuration after the processing: get 3g and process rear pedotheque, add the 1:1(volume ratio of 10mL), ultrasonic extraction 10 minutes, centrifugal, the collection supernatant, add extract again, repeats 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured, and result is 265.6 mg/kg.
5, biologically effective state polycyclic aromatic hydrocarbon content calculating: contain=432.4-265.6=166.8mg/kg of palycyclic aromatic after polycyclic aromatic hydrocarbon content before biologically effective state polycyclic aromatic hydrocarbon content=processing-processing accounts for and processes 38.6% of front polycyclic aromatic hydrocarbon content.
6, test result checking: get 5g drying and screening pedotheque, add K
2s
2o
8and deionized water, S
2o
8 2-with organic ratio be 12g/g, persulfate concentration is 0.0357g/ml, at 70 ℃ of lower shaking water bath 3h(120rpm), by the sample filtering of processing, get 3g, the 1:1(volume ratio that adds 10mL) methylene chloride and acetone hybrid extraction liquid, ultrasonic extraction 10 minutes, centrifugal, collect supernatant, again add extract, repeat 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured and is adopted the acetone solvent extraction to measure polycyclic aromatic hydrocarbon content, and result is 274.8 mg/kg.Polycyclic aromatic hydrocarbon content=432.4-274.8=157.6mg/kg after polycyclic aromatic hydrocarbon content-oxidation processes before biologically effective state polycyclic aromatic hydrocarbon content=oxidation processes, account for and process 36.4% of front polycyclic aromatic hydrocarbon content.
7, by step 5 and step 6 test result, can find out, only differ 2.2% based on biologically effective state polycyclic aromatic hydrocarbon content in thermal desorption processing mensuration soil and based on biologically effective state polycyclic aromatic hydrocarbon content result in persulfate oxidation processing mensuration soil, show to process based on thermal desorption the method accuracy of measuring biologically effective state polycyclic aromatic hydrocarbon content higher, test result is credible.
Embodiment 2:
1, the preparation of pedotheque: sample collection is from certain coke-oven plant's Polluted Soil, and polycyclic aromatic hydrocarbon content is higher.The pedotheque natural air drying that to gather, the soil after air-dry grinds and crosses 20 mesh sieves, and collecting sieves sieves for next step.
2, methylene chloride and acetone hybrid extraction liquid polycyclic aromatic hydrocarbon content mensuration before the processing: get 3g drying and screening pedotheque, add the 1:1(volume ratio of 10mL), ultrasonic extraction 10 minutes, centrifugal, collect supernatant, again add extract, repeat 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured, and result is 1833.6mg/kg.
3, thermal desorption is processed: get 100g drying and screening pedotheque, soil sample is put into to Soil Thermal desorption rotary furnace (Soil Thermal desorption rotary furnace test macro, the patent No.: ZL 2,012 2 0468562.5) Quartz stove tube in, with the stove hook, soil sample is shifted onto to the constant temperature zone position of Quartz stove tube middle, then install flange, open carrier gas, regulate Soil Thermal desorption rotary furnace test macro, be 30min heat time heating time, and heating-up temperature is 250 ℃.After heating finishes, continue logical carrier gas cooling to soil sample, then close carrier gas, the outlet side of unloading the pipe type rotary furnace is connected with the flange of the air pressure valve of giving vent to anger, adjust the Quartz stove tube inclination angle, make soil sample from landing in Quartz stove tube, by soil sample collection (Soil Thermal desorption rotary furnace test macro and method of testing thereof, application number: 201210340236.0).
4, methylene chloride and acetone hybrid extraction liquid polycyclic aromatic hydrocarbon content mensuration after the processing: get 3g and process rear pedotheque, add the 1:1(volume ratio of 10mL), ultrasonic extraction 10 minutes, centrifugal, the collection supernatant, add extract again, repeats 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured, and result is 722.1 mg/kg.
5, biologically effective state polycyclic aromatic hydrocarbon content calculates: polycyclic aromatic hydrocarbon content=1833.6-722.1=1111.5mg/kg after polycyclic aromatic hydrocarbon content before biologically effective state polycyclic aromatic hydrocarbon content=processing-processing accounts for and processes 60.6% of front polycyclic aromatic hydrocarbon content.
6, test result checking: get 5g drying and screening pedotheque, add K
2s
2o
8and deionized water, S
2o
8 2-with organic ratio be 12g/g, persulfate concentration is 0.0357g/ml, at 70 ℃ of lower shaking water bath 3h(120rpm), by the sample filtering of processing, get 3g, the 1:1(volume ratio that adds 10mL) methylene chloride and acetone hybrid extraction liquid, ultrasonic extraction 10 minutes, centrifugal, collect supernatant, again add extract, repeat 5 times.Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, crosses 0.22
the m miillpore filter, high performance liquid chromatograph (HPLC) is measured and is adopted the acetone solvent extraction to measure polycyclic aromatic hydrocarbon content, result is 733.2 mg/kg, polycyclic aromatic hydrocarbon content=1833.6-733.2=1100.4mg/kg after polycyclic aromatic hydrocarbon content-oxidation processes before biologically effective state polycyclic aromatic hydrocarbon content=oxidation processes, account for and process 60.0% of front polycyclic aromatic hydrocarbon content.
7, by step 5 and step 6 test result, can find out, only differ 0.6% based on biologically effective state polycyclic aromatic hydrocarbon content in thermal desorption processing mensuration soil and based on biologically effective state polycyclic aromatic hydrocarbon content result in persulfate oxidation processing mensuration soil, show to process based on thermal desorption the method accuracy of measuring biologically effective state polycyclic aromatic hydrocarbon content higher, test result is credible.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (4)
1. a method that process to measure biologically effective state polycyclic aromatic hydrocarbon content in soil based on thermal desorption, it is characterized in that: pedotheque to be measured is divided into to two parts, the a acetone solvent extraction that adopts is measured the front polycyclic aromatic hydrocarbon content of processing, another part is first processed and is removed biologically effective state palycyclic aromatic in sample through thermal desorption, polycyclic aromatic hydrocarbon content after adopting afterwards the acetone solvent extraction measure to process, the polycyclic aromatic hydrocarbon content difference by twice mensuration draws biologically effective state polycyclic aromatic hydrocarbon content in pedotheque.
2. the method for claim 1, it is characterized in that: the concrete steps of the method are:
(1) pedotheque preparation: by the pedotheque natural air drying, the soil after air-dry grinds and crosses 20 mesh sieves, and collecting sieves sieves for next step;
(2) processing front polycyclic aromatic hydrocarbon content measures: get 3g drying and screening pedotheque, add methylene chloride and acetone hybrid extraction liquid that the 10mL volume ratio is 1:1, and ultrasonic extraction 10 minutes, centrifugal, collect supernatant, again add extract, repeat 5 times;
Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, is crossed 0.22 μ m miillpore filter, then with high performance liquid chromatograph, measures polycyclic aromatic hydrocarbon content;
(3) thermal desorption is processed: get 100g drying and screening pedotheque, soil sample is put into to the Quartz stove tube of Soil Thermal desorption rotary furnace, with the stove hook, soil sample is shifted onto to the constant temperature zone position of Quartz stove tube middle, then install flange, open carrier gas, regulate Soil Thermal desorption rotary furnace test macro, be 20-40min heat time heating time, and heating-up temperature is 150-300 ℃;
After heating finishes, continue logical carrier gas cooling to soil sample, then close carrier gas, the outlet side of unloading the pipe type rotary furnace is connected with the flange of the air pressure valve of giving vent to anger, and adjustment Quartz stove tube inclination angle makes soil sample from landing in Quartz stove tube, by soil sample collection;
(4) processing rear polycyclic aromatic hydrocarbon content measures: get 3g and process rear pedotheque, add methylene chloride and acetone hybrid extraction liquid that the 10mL volume ratio is 1:1, and ultrasonic extraction 10 minutes, centrifugal, collect supernatant, again add extract, repeat 5 times;
Extract anhydrous sodium sulfate filtration drying, the Rotary Evaporators evaporate to dryness, methanol constant volume, to 2mL, is crossed 0.22 μ m miillpore filter, then with high performance liquid chromatograph, measures polycyclic aromatic hydrocarbon content;
(5) biologically effective state polycyclic aromatic hydrocarbon content calculates: polycyclic aromatic hydrocarbon content after the processing that before the processing that biologically effective state polycyclic aromatic hydrocarbon content=step (2) records, polycyclic aromatic hydrocarbon content-step (4) records.
3. method as claimed in claim 2 is characterized in that: in step (3), be 30min heat time heating time.
4. the method for claim 1 is characterized in that: in step (3), heating-up temperature is 200-250 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467040A (en) * | 2015-12-30 | 2016-04-06 | 乌鲁木齐谱尼测试科技有限公司 | Method for detecting residual quantity of aminoanisole and paranitroanisole in soil |
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|---|---|---|---|---|
| EP0952134A1 (en) * | 1998-04-21 | 1999-10-27 | Menyes, Ulf, Dr. | Process for the separation of polycyclic aromatic hydrocarbons by chromatography |
| EP2087947A2 (en) * | 2008-02-08 | 2009-08-12 | Depuracque Sviluppo S.R.L. | Method for reclaiming soil, sediment and sludge dredged from watercourses contaminated by heavy metals and by dangerous and toxic organic compounds |
| CN101706480A (en) * | 2009-11-27 | 2010-05-12 | 沈阳大学 | Method for analyzing polycyclic aromatic hydrocarbon content of soil |
| CN102818816A (en) * | 2012-09-14 | 2012-12-12 | 北京市环境保护科学研究院 | Soil thermal desorption rotary furnace testing system and testing method thereof |
| KR101301218B1 (en) * | 2012-09-14 | 2013-08-28 | 아름다운 환경건설(주) | System of decontaminating soils |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0952134A1 (en) * | 1998-04-21 | 1999-10-27 | Menyes, Ulf, Dr. | Process for the separation of polycyclic aromatic hydrocarbons by chromatography |
| EP2087947A2 (en) * | 2008-02-08 | 2009-08-12 | Depuracque Sviluppo S.R.L. | Method for reclaiming soil, sediment and sludge dredged from watercourses contaminated by heavy metals and by dangerous and toxic organic compounds |
| CN101706480A (en) * | 2009-11-27 | 2010-05-12 | 沈阳大学 | Method for analyzing polycyclic aromatic hydrocarbon content of soil |
| CN102818816A (en) * | 2012-09-14 | 2012-12-12 | 北京市环境保护科学研究院 | Soil thermal desorption rotary furnace testing system and testing method thereof |
| KR101301218B1 (en) * | 2012-09-14 | 2013-08-28 | 아름다운 환경건설(주) | System of decontaminating soils |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467040A (en) * | 2015-12-30 | 2016-04-06 | 乌鲁木齐谱尼测试科技有限公司 | Method for detecting residual quantity of aminoanisole and paranitroanisole in soil |
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Application publication date: 20131211 |