CN102721767A - Method for separating and analyzing polyethylene residues in soil environment - Google Patents
Method for separating and analyzing polyethylene residues in soil environment Download PDFInfo
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- CN102721767A CN102721767A CN2012101533485A CN201210153348A CN102721767A CN 102721767 A CN102721767 A CN 102721767A CN 2012101533485 A CN2012101533485 A CN 2012101533485A CN 201210153348 A CN201210153348 A CN 201210153348A CN 102721767 A CN102721767 A CN 102721767A
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Abstract
The present invention relates to a method for separating and analyzing polyethylene residues in a soil environment. The method includes the following steps of: adding a certain amount of a pretreated soil sample into a beaker; adding inorganic acid or inorganic mixed acid into the beaker according to a certain proportion for reactions respectively in a static condition and a stirring condition at room temperature with each reaction time being 10 to 50 minutes; adding distilled water and allowing the mixture to stand for 8 to 12 hours; shifting an upper layer liquid to a separatory funnel and discarding a lower layer of a water phase; using water and ethanol to respectively wash residues for 2 to 3 times; shifting the washed residues to the beaker for further washing the washed residues for 2 to 10 minutes by successively using 0.5 mol/L to 5 mol/L of sodium hydroxide and 0.5 mol/L to 5 mol/L of hydrochloric acid at the temperature from 30 DEC C to 50 DEG C; again shifting the mixture to the separatory funnel and discarding a lower layer of a water phase; washing residues until filtrate becomes neutral; using tetrahydrofuran to soak and wash the residues for 2 to 10 minutes; and leaching the residues and drying filtrate to obtain a certain amount of the polyethylene residues. Molecular weight and molecular weight distribution of the residues are determined by using a gel permeation chromatography.
Description
Technical field
The present invention relates to the method for separating and analyzing of tygon residue in a kind of soil environment, belong to the Environmental Analytical Chemistry technical field.
Background technology
Panoramic plastic products have greatly enriched people's life, but because plastics are being difficult to degraded under the nature condition, thereby have caused serious " white pollution ".Countries in the world have all taked multiple means to solve the pollution problem of plastic refuse, bury like soil, burn, and reclaim, but all there is certain drawback in these methods.For thoroughly solving this difficult problem, the research of degradation plastic has become the domestic and international research focus.Wherein tygon is the maximum kind of output in world's plastics variety, and its application surface is also the widest, accounts for 1/3 of world's plastics total production, and present poly output has reached 8,000 ten thousand tons, and the industrialization in existing 70 years is historical.Degradation process and mechanism of degradation for the tygon discarded object; And to the influences of soil and crops; Scholar both domestic and external did a large amount of research; But it is residual generally to take the soil landfill method to follow the tracks of the polyethylene ground film bulk; Or mulch film is administered to the field, or under laboratory condition microbe inoculation simulation field condition, during constantly gather the ground membrane sample; Indexs such as variation of test surfaces proterties and growth of microorganism rank, mass loss, pulling strengrth, breaking elongation, structural change, oxidative degradation degree, molecular weight variation, surface structure variation, oxygen consumed tolerance, carbon dioxide production, thus the possible reactions step of polyethylene ground film degraded and the time of degrading fully and need spend calculated.
From the former study report, can see that degradable polyethylene product such as mulch film can be degraded into fragment or Powdered in short-term with mulch film under ambient light, temperature, water, gas, the coefficient environment of microorganism, eliminated " visual pollution ".Think these tygon fragments or powder in the past to crops and not influence of environment, and think that it is degraded fully.After tygon pulverize powder got into soil so, fully whether it degraded, and perhaps how long degraded also needs fully, just has no idea to have known.For degraded situation and the degradation time behind the residual body entering of the true objective evaluation degradable polyethylene plastics soil; The present invention is according to tygon and soil physicochemical property separately; Adopt separation and concentration and relevant detection means; Set up the technical method of compartment analysis tygon residue from soil environment, this has not only enlarged the scope that organic contaminant detects in the environment, and the research that can be the evaluation of tygon environment degradable simultaneously provides a kind of new means.
Summary of the invention
Goal of the invention
The method for separating and analyzing that the purpose of this invention is to provide tygon residue in a kind of soil environment; Mainly be that principal ingredient monox according to soil can be dissolved in some mineral acid; And the tygon chemical stability is good, and the erosion of the most of soda acids of ability (not anti-acid with oxidizing property) is insoluble to common solvent under the normal temperature; Thereby make most of soil particle dissolving; Then coagulation is at container bottom for the undissolvable soil of fraction, and density of pe gentlier gets into liquid phase, carries out Separation of Solid and Liquid with separating funnel; Respectively with certain reagent wash supernatant liquid improving poly purity, sampling is with its molecular weight of gel permeation chromatography and molecular weight distribution from clean solution; The surplus solution suction filtration places double dish, oven dry, and metering can obtain tygon residual quantity in the soil environment, and the method can apply to the separation and Extraction and the detection of tygon residue in the various soil environments.
Technical scheme
The method for separating and analyzing of tygon residue in a kind of soil environment, mainly comprise following five steps: fetch earth earth sample, oven dry, pulverizing obtain soil sample behind the mixing; Get a certain amount of soil sample and place polytetrafluoroethylene beaker, add soil sample: solution weight is than the mineral acid or the inorganic nitration mixture of 1:4～8 times, and room temperature reaction 10～50 minutes on the magnetic stirring apparatus continued stirring reaction 10～50 minutes in the fuming cupboard; Add distilled water, left standstill 8～12 hours, change supernatant liquid over to separating funnel; Discard lower floor's water, first water, ethanol difference debris 2～3 times change in the beaker; Successively NaOH, the 0.5mol/L～5mol/L hydrochloric acid with 0.5mol/L～5mol/L respectively washed 2～10 minutes for 30～50 ℃, changed separating funnel once more over to, discarded lower floor's water; Residue washing to filtrating is neutral, tetrahydrofuran washing by soaking 2～10 minutes, suction filtration; Filtrating places double dish, oven dry, and metering can obtain the amount of tygon residue in the soil; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
Soil is selected one or more the combination in any in sand, loam, the clay for use.
Mineral acid is a hydrofluorite, and inorganic nitration mixture is that (volume ratio is the potpourri of 5:1～5:5) for hydrofluorite and hydrochloric acid.
Beneficial effect
The research of degradation plastic has become the domestic and international research focus, and in order to estimate the degradation property of degradation plastic, various countries all drop into definition, experimental evaluation method and the Study on standards formulation work that bigger human and material resources, financial resources are devoted to degradative plastics.But the evaluation criterion of existing domestic and international degradative plastics or the foundation of degradation property method all are the experimental evaluation methods that experiment material is placed laboratory manual simulation's natural conditions; It all is the degradation property of estimating plastics through the investigation of single factors; But in fact degradative plastics is degraded in physical environment and will be received the influence of several factors, like microorganism in heat, oxygen, humidity, pressure, biomacromolecule, ultraviolet light and the soil etc.
Be degraded into the powder situation of change behind the soil of going forward side by side to the degradable polyethylene mulch film; The Tissuemat E powder of different molecular weight added to adopt the separation and concentration means to reclaim Tissuemat E in the soil again; Detect its molecular weight distribution and the recovery and carry out the investigation of degradation behavior; For setting up the new degrading polyethylene plastics evaluation method of a cover possibility is provided, makes it more truly reflect polyethylene ground film more objectively in the degradation in soil situation, this method is not all seen bibliographical information both at home and abroad.The device that the present invention uses is simple, easy to operate, and extraction ratio is stable, and average extraction ratio can reach more than 80%, is applicable to the separation and Extraction and the detection of tygon residue in the various soil environments.
Embodiment
Embodiment 1: get 500 g sand samples, oven dry, pulverizing obtain soil sample behind the mixing; Get the 10g soil sample in 500 mL polytetrafluoroethylene beakers; Add solution weight than being the inorganic nitration mixture of 1:5 (hydrofluorite and hydrochloric acid volume ratio are 5:1); Room temperature reaction is 15 minutes in the fuming cupboard, and magnetic stirring apparatus continued stirring reaction about 20 minutes, no longer dissolved until soil; Left standstill 12 hours; Supernatant liquid is transferred in the 500 mL separating funnels, discards lower floor's water, first water, ethanol difference debris 2 times change in the beaker; Successively NaOH, the 3mol/L hydrochloric acid with 4mol/L respectively washed 10 minutes for 35 ℃, changed separating funnel once more over to, discarded lower floor's water, and residue washing to filtrating is neutral; Tetrahydrofuran washing by soaking 10 minutes, suction filtration, filtrating places double dish; Oven dry, metering can obtain the amount of tygon residue in the soil, and extraction ratio is 82.62%; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
Embodiment 2: get 300g loam sample, oven dry, pulverizing obtain soil sample behind the mixing; Get the 5g soil sample in 500 mL polytetrafluoroethylene beakers, add solution weight than being the mineral acid of 1:4 (hydrofluorite), room temperature reaction is 10 minutes in the fuming cupboard, and magnetic stirring apparatus continued stirring reaction about 10 minutes, no longer dissolved until soil; Left standstill 11 hours; Supernatant liquid is transferred in the 500 mL separating funnels, discards lower floor's water, first water, ethanol difference debris 2 times change in the beaker; Successively NaOH, the 5mol/L hydrochloric acid with 5mol/L washed 6 minutes for 30 ℃, changed separating funnel once more over to, discarded lower floor's water, and residue washing to filtrating is neutral; Tetrahydrofuran washing by soaking 6 minutes, suction filtration, filtrating places double dish; Oven dry, metering can obtain the amount of tygon residue in the soil, and extraction ratio is 84.31%; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
Embodiment 3: get the 400g clay sample, oven dry, pulverizing obtain soil sample behind the mixing; Get the 30g soil sample in 1000 mL polytetrafluoroethylene beakers; Add solution weight than being the inorganic nitration mixture of 1:7 (hydrofluorite and hydrochloric acid volume ratio are 5:3); Room temperature reaction is 50 minutes in the fuming cupboard, and magnetic stirring apparatus continued stirring reaction about 40 minutes, no longer dissolved until soil; Left standstill 10 hours; Supernatant liquid is transferred in the 1000mL separating funnel, discards lower floor's water, first water, ethanol difference debris 3 times change in the beaker; Successively NaOH, the 4mol/L hydrochloric acid with 2mol/L washed 8 minutes for 45 ℃, changed separating funnel once more over to, discarded lower floor's water, and residue washing to filtrating is neutral; Tetrahydrofuran washing by soaking 8 minutes, suction filtration, filtrating places double dish; Oven dry, metering can obtain the amount of tygon residue in the soil, and extraction ratio is 80.31%; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
Embodiment 4: get 200g clay sample and 100g sand sample, oven dry, pulverizing obtain soil sample behind the mixing; Get the 20g soil sample in 1000 mL polytetrafluoroethylene beakers, add solution weight than being the mineral acid of 1:6 (hydrofluorite), room temperature reaction is 30 minutes in the fuming cupboard, and magnetic stirring apparatus continued stirring reaction about 40 minutes, no longer dissolved until soil; Left standstill 9 hours; Supernatant liquid is transferred in the 1000mL separating funnel, discards lower floor's water, first water, ethanol difference debris 3 times change in the beaker; Successively NaOH, the 2 mol/L hydrochloric acid with 1mol/L washed 4 minutes for 40 ℃, changed separating funnel once more over to, discarded lower floor's water, and residue washing to filtrating is neutral; Tetrahydrofuran washing by soaking 4 minutes, suction filtration, filtrating places double dish; Oven dry, metering can obtain the amount of tygon residue in the soil, and extraction ratio is 86.31%; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
Embodiment 5: get 100g sand sample and 200g loam sample, oven dry, pulverizing obtain soil sample behind the mixing; Get the 10g soil sample in 500 mL polytetrafluoroethylene beakers, add solution weight than being the mineral acid of 1:5 (hydrofluorite), room temperature reaction is 20 minutes in the fuming cupboard, and magnetic stirring apparatus continued stirring reaction about 30 minutes, no longer dissolved until soil; Left standstill 8 hours; Supernatant liquid is transferred in the 500 mL separating funnels, discards lower floor's water, first water, ethanol difference debris 2 times change in the beaker; Successively NaOH, the 0.5mol/L hydrochloric acid with 0.5mol/L washed 2 minutes for 35 ℃, changed separating funnel once more over to, discarded lower floor's water, and residue washing to filtrating is neutral; Tetrahydrofuran washing by soaking 2 minutes, suction filtration, filtrating places double dish; Oven dry, metering can obtain the amount of tygon residue in the soil, and extraction ratio is 86.31%; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
Embodiment 6: get 200g loam sample and 200g clay sample, oven dry, pulverizing obtain soil sample behind the mixing; Get the 40g soil sample in 1000 mL polytetrafluoroethylene beakers; Add solution weight than being the inorganic nitration mixture of 1:8 (hydrofluorite and hydrochloric acid volume ratio are 5:5); Room temperature reaction is 50 minutes in the fuming cupboard, and magnetic stirring apparatus continued stirring reaction about 50 minutes, no longer dissolved until soil; Left standstill 10 hours; Supernatant liquid is transferred in the 1000mL separating funnel, discards lower floor's water, first water, ethanol difference debris 3 times change in the beaker; Successively NaOH, the 1mol/L hydrochloric acid with 3mol/L washed 5 minutes for 50 ℃, changed separating funnel once more over to, discarded lower floor's water, and residue washing to filtrating is neutral; Tetrahydrofuran washing by soaking 5 minutes, suction filtration, filtrating places double dish; Oven dry, metering can obtain the amount of tygon residue in the soil, and extraction ratio is 81.62%; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
Claims (3)
1. the method for separating and analyzing of tygon residue in the soil environment is characterized in that, mainly comprises following five steps:
Fetch earth earth sample, oven dry, pulverizing obtain soil sample behind the mixing; Get a certain amount of soil sample and place polytetrafluoroethylene beaker, add soil sample: solution weight is than the mineral acid or the inorganic nitration mixture of 1:4～8 times, and room temperature reaction 10～50 minutes on the magnetic stirring apparatus continued stirring reaction 10～50 minutes in the fuming cupboard; Add distilled water, left standstill 8～12 hours, change supernatant liquid over to separating funnel; Discard lower floor's water, water, ethanol difference debris 2～3 times change in the beaker; Successively NaOH, the 0.5 mol/L～5 mol/L hydrochloric acid with 0.5 mol/L～5 mol/L respectively washed 2～10 minutes for 30～50 ℃, changed separating funnel once more over to, discarded lower floor's water; Residue washing to filtrating is neutral, tetrahydrofuran washing by soaking 2～10 minutes, suction filtration; Filtrating places double dish, oven dry, and metering can obtain the amount of tygon residue in the soil; Its molecular weight of gel permeation chromatography and molecular weight distribution are adopted in sampling.
2. according to the method for separating and analyzing of tygon residue in a kind of soil environment described in the claim 1, it is characterized in that described soil is one or more the combination in any in sand, loam, the clay.
3. according to the method for separating and analyzing of tygon residue in a kind of soil environment described in the claim 1, it is characterized in that said mineral acid is a hydrofluorite, inorganic nitration mixture is that (volume ratio is the potpourri of 5:1～5:5) for hydrofluorite and hydrochloric acid.
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| CN2012101533485A CN102721767A (en) | 2012-05-17 | 2012-05-17 | Method for separating and analyzing polyethylene residues in soil environment |
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| CN2012101533485A CN102721767A (en) | 2012-05-17 | 2012-05-17 | Method for separating and analyzing polyethylene residues in soil environment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102890132A (en) * | 2012-10-19 | 2013-01-23 | 西南科技大学 | Method for detecting polyethylene residual quantity in soil environment by using Soxhlet extraction method |
| CN104007039A (en) * | 2014-05-30 | 2014-08-27 | 甘肃省农业科学院农业经济与信息研究所 | Method for monitoring mulching film residue pollution coefficient of surface soil |
| CN107413833A (en) * | 2017-07-25 | 2017-12-01 | 中国科学院新疆生态与地理研究所 | The micro- plastics separation method of agricultural land soil polyethylene disperseed based on high-shear emulsifying |
| CN112005094A (en) * | 2018-03-07 | 2020-11-27 | 玛格丽特·安娜·莱蒂齐娅·费兰特 | Method for extracting and measuring micro-plastics in sample containing organic and inorganic matrix |
-
2012
- 2012-05-17 CN CN2012101533485A patent/CN102721767A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| EMO CHIELLINI等: "Biodegradation of thermally-oxidized, fragmented low-density polyethylenes", 《POLYMER DEGRADATION AND STABILITY》 * |
| PETER P. KLEMCHUK: "Degradable Plastics: A Critical Review", 《POLYMER DEGRADATION AND STABILITY》 * |
| 何晶: "不同分子量的聚乙烯粉末对土壤环境及作物生长的影响研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102890132A (en) * | 2012-10-19 | 2013-01-23 | 西南科技大学 | Method for detecting polyethylene residual quantity in soil environment by using Soxhlet extraction method |
| CN104007039A (en) * | 2014-05-30 | 2014-08-27 | 甘肃省农业科学院农业经济与信息研究所 | Method for monitoring mulching film residue pollution coefficient of surface soil |
| CN107413833A (en) * | 2017-07-25 | 2017-12-01 | 中国科学院新疆生态与地理研究所 | The micro- plastics separation method of agricultural land soil polyethylene disperseed based on high-shear emulsifying |
| CN107413833B (en) * | 2017-07-25 | 2019-11-08 | 中国科学院新疆生态与地理研究所 | The micro- plastics separation method of agricultural land soil polyethylene based on high-shear emulsifying dispersion |
| CN112005094A (en) * | 2018-03-07 | 2020-11-27 | 玛格丽特·安娜·莱蒂齐娅·费兰特 | Method for extracting and measuring micro-plastics in sample containing organic and inorganic matrix |
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Application publication date: 20121010 |