CN106053766A - Method for quickly determining content of sodium peroxydisulfate in soil - Google Patents

Method for quickly determining content of sodium peroxydisulfate in soil Download PDF

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Publication number
CN106053766A
CN106053766A CN201610599894.XA CN201610599894A CN106053766A CN 106053766 A CN106053766 A CN 106053766A CN 201610599894 A CN201610599894 A CN 201610599894A CN 106053766 A CN106053766 A CN 106053766A
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China
Prior art keywords
soil
sodium peroxydisulfate
measured
content
mud
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CN201610599894.XA
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CN106053766B (en
Inventor
王文坦
邵雁
李社锋
陶玲
郭华军
赵波
宋自新
康健
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Duhuan Testing Wuhan Co ltd
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China City Environment Protection Engineering Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24Earth materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration

Abstract

The invention provides a method for quickly determining the content of sodium peroxydisulfate in soil. The method comprises the following steps: (1) measuring the moisture content of soil to be measured; (2) calculating the mass of the dry basis of the soil to be measured according to the moisture content, and supplementing deionized water into the soil to be measured to obtain mud; (3) taking the mud in the step (2), adding dilute sulfuric acid, mixing, and stirring evenly; (4) adding ferrous salt in mixed liquor in the step (3), mixing and stirring; (5) titrating the reacted mixed liquor in the step (4) by a potassium permanganate solution till the solution becomes light pink, and determining the volume of the consumed potassium permanganate solution; and (6) calculating the content of sodium peroxydisulfate in the soil to be measured. In the method for quickly determining the content of sodium peroxydisulfate in soil, the number of used reagents is small, test time is short, the cost is low, and a test process is convenient and speedy; and the method can be used in a polluted place on the spot.

Description

A kind of method of sodium peroxydisulfate content in quick mensuration soil
Technical field
The invention belongs to technical field of soil remediation, be specifically related to the side of sodium peroxydisulfate content in a kind of quick mensuration soil Method.
Background technology
Along with development and the quickening of Development of China's Urbanization of China's industrial or agricultural, along with adjustment and the urbanization of Industry Structure The quickening of process, the big and medium-sized cities in the whole nation all implement " move back two and enter three ", the policy in " Tui Chengjin garden ", large quantities of relate to chemical industry, smelting The successively resettlement of the contaminating enterprises of the industries such as gold, oil, transportation, light industry or closedown.Place is left in the resettlement of a lot of industrial undertakings Soil present in a large amount of organic pollutions, these pollutant constantly migrate and convert, can pass through gas-soil circulate with water- Soil is recycled in other surrounding mediums, it is also possible to directly enter human body by food chain or human breathing, and the harm mankind are good for Health.
Chemical oxidation techniques is conventional a kind of recovery technique for organic polluted soil, and this technology is mainly by oozing Penetrate into oxidation reaction produced by the chemical oxidizing agent in soil and pollutant, make contaminant degradation or be converted into low toxicity, low shifting The product of dynamic property.Sodium peroxydisulfate is a kind of effective chemical oxidation medicament in chemical oxidation recovery technique, quickly measures in soil The content of sodium peroxydisulfate, contributes to the consumption of sodium peroxydisulfate in analysis and assessment soil, and then assessment chemical oxidation techniques Chinese medicine The use dosage of agent.GB GB/T 23940-2009 only describes the analysis method of sodium peroxydisulfate powder, but the method Needing to add more reagent, the testing time is longer, there is inconvenience in contaminated site onsite application the method.
Summary of the invention
It is an object of the invention to overcome sodium peroxydisulfate in existing soil to analyze method need to add more reagent, testing time Longer, in the problem that contaminated site onsite application exists inconvenience.
To this end, the invention provides a kind of method of sodium peroxydisulfate content in quick mensuration soil, comprise the steps:
1) the moisture content w of soil butt to be measured is measured.
2) according to step 1) in the moisture content that records to calculate the quality of soil butt to be measured be m1, supplement in soil to be measured Deionized water, making volume is V1Mud.
3) take the step 2 that volume is V) in mud, add dilute sulfuric acid mixing, stir.
4) to step 3) mixed liquor in add quality be m2Ferrous salt, mix and blend reacts a period of time.
5) by the potassium permanganate solution titration step 4 that concentration is c) in reacted mixed solution, until solution becomes shallow Till pink colour, the potassium permanganate solution volume of consumption is V2
6) sodium peroxydisulfate content in soil butt to be measured is calculated:
Further, above-mentioned steps 1) in soil to be measured moisture content use oven drying method measure.
Further, above-mentioned steps 2) in pedotheque to be measured be initial soil sample.
Further, above-mentioned steps 2) in the mass fraction of mud for preparing be 10~60%.
It is further preferred that above-mentioned steps 2) in the mass fraction of mud for preparing be 50%.
Further, above-mentioned steps 3) in the mass fraction of dilute sulfuric acid that adds be 20~40%.
Further, above-mentioned steps 4) in ferrous salt be ferrous sulfate, ferrous sulfate hydrate, Ferrous ammonium sulfate, sulphuric acid Ferrous ammonium hydrate or ferrous chloride.
Further, above-mentioned steps 4) in mix and blend reaction time be 5~15 minutes.
Further, above-mentioned pedotheque to be measured is arranged organizes parallel laboratory test more, and in soil, sodium peroxydisulfate is flat containing measuring many groups The meansigma methods of row experiment.
In soil of the present invention, the reaction mechanism of sodium peroxydisulfate content assaying method is as follows:
(1) ferrous salt is reacted with sodium peroxydisulfate in soil;Wherein, ferrous salt excess so that the sodium peroxydisulfate in soil is complete Full response, reaction equation is as follows:
2Fe2++S2O8 2-→2Fe3++2SO4 2-
(2) ferrous salt of acid potassium permanganate overtitration, reaction equation is as follows:
5Fe2++MnO4 -+8H+→5Fe3++Mn2++4H2O。
Compared with prior art, beneficial effects of the present invention:
(1) present invention provide this quick mensuration soil in sodium peroxydisulfate content method employed in reagent few, Testing time is short, low cost, and test process is convenient and swift, is conducive at contaminated site field conduct.
(2) in this quick mensuration soil that the present invention provides, in the method for sodium peroxydisulfate content, ferrous salt can be according to reality Border situation has multiple choices, applied widely.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment It is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area All other embodiments that art personnel are obtained under not making creative work premise, broadly fall into the model of present invention protection Enclose.
Embodiment 1:
Present embodiments provide a kind of method of sodium peroxydisulfate content in quick mensuration soil, comprise the steps:
1) the moisture content ω of soil butt to be measured is measured;In soil, moisture content can select oven drying method to be measured, and dries Method measures simple direct, and it specifically measures process is prior art, is not described in detail in the present embodiment.
2) according to step 1) in the moisture content ω that records to calculate the quality of soil butt to be measured be m1, mend in soil to be measured Filling deionized water, making volume is V1Mud.
Wherein, quality m of soil butt to be measured1=m/ (1+ ω), m is the quality of soil to be measured, to be measured in this step Soil is the primary sample soil not doing any process, step 1) in after the pedotheque measuring moisture content is not useable for Continuous step.So that subsequent reactions can be smoothed out, the mass fraction of described prepared mud is 10~60%, if added water Measuring very few, mud is feeding-up, and soil dispersion is not opened, and is unfavorable for that sodium peroxydisulfate is uniformly distributed in mud, the more polydispersion that the water yield adds The most uniform, but make the lowest subsequent detection that is unfavorable for of sodium peroxydisulfate concentration too much, the quality of preferred mud in the present embodiment Mark is 50%.
3) take the step 2 that volume is V) in mud, add dilute sulfuric acid mixing, stir;Wherein, dilute sulfuric acid is follow-up Reaction provides sour environment, and the mass fraction of the dilute sulfuric acid of addition is 20~40%, and its volume is with specific reference to the mud taken Depending on amount.
4) to step 3) mixed liquor in add quality be m2Ferrous salt, mix and blend reacts a period of time, to mud In sodium peroxydisulfate react completely, it is however generally that, mix and blend reaction time be that 5~15 minutes sodium peroxydisulfates can react Entirely.Ferrous salt is reacted with sodium peroxydisulfate in soil as reaction reagent, and the ferrous salt herein added wants excess so that in soil Sodium peroxydisulfate can react completely, and ferrous salt can have multiple choices according to practical situation, and in the present embodiment, ferrous salt can be Ferrous sulfate, ferrous sulfate hydrate, Ferrous ammonium sulfate, Ferrous ammonium sulfate hydrate or ferrous chloride.
5) by the potassium permanganate solution titration step 4 that concentration is c) in reacted mixed solution, until solution becomes shallow Till pink colour, the potassium permanganate solution volume of consumption is V2.Potassium permanganate in this step is used for titrating step under sour environment Rapid 4) ferrous salt of excess in, so that it is determined that step 4) in the amount of ferrous salt reacted with sodium peroxydisulfate in soil.
6) according to the proportionate relationship that reactant in the consumption of each reagent of said determination and reaction equation is corresponding, soil to be measured is calculated Sodium peroxydisulfate content in earth butt:Wherein, m1For soil to be measured The quality of butt, g;m2The quality of the ferrous salt for adding, g;MFerrous saltMolal weight for selected ferrous salt;C is Gao Meng The concentration of acid potassium solution, mol/L;V1For quality m1The cumulative volume of the mud that soil butt to be measured prepares, ml;V2For potassium permanganate The volume of solution consumption, L;V is the volume of the mud for experiment, ml.
In this quick mensuration soil that the present invention provides, the reagent employed in the method for sodium peroxydisulfate content is few, test Time is short, low cost, and test process is convenient and swift, is conducive at contaminated site field conduct.
Embodiment 2:
In the mensuration soil of the present embodiment employing embodiment 1, the method for sodium peroxydisulfate content is specifically to the mistake in the soil of somewhere Sodium sulphate content is measured, and detailed process is as follows:
(1) taking part pedotheque to be measured, the moisture content ω measuring soil butt to be measured is 25%.
(2) separately taking the original soil to be measured of m=10g, and supplement 6ml deionized water wherein, prepared mass fraction is 50% Mud (on the basis of the butt quality removing moisture content), stir, the cumulative volume V of mud1=16ml, soil dry to be measured Substrate amount m1=m/ (1+ ω)=8g.
(3) arranging three groups of parallel laboratory tests, often group parallel laboratory test is all from step 2) mud prepared takes V=5ml stirring all Even mud, and to often organizing, parallel laboratory test adds the dilute sulfuric acid 25ml that mass fraction is 25%, stir 2 minutes.
(4) to step 3) the mixed solution often organizing parallel laboratory test in all add m2Dried seven hydrated sulfuric acid of=2g are sub- Ferrum (FeSO4·7H2O), continuing stirring 10 minutes, the sodium peroxydisulfate reaction in soil is completely.
(5) by the potassium permanganate solution titration step 4 of concentration c=0.1mol/L) in mixed liquor in three groups of parallel laboratory tests, Till solution colour becomes lightpink, the titer of three groups of parallel laboratory test potassium permanganate solutions be respectively 0.014L, 0.015L, 0.014L, the then quantification of 0.014L of the mean droplet of three groups of parallel laboratory tests.
(6) sodium peroxydisulfate content in soil to be measured is calculated
Exemplified as above is only the illustration to the present invention, is not intended that the restriction to protection scope of the present invention, all It is within design same or analogous with the present invention belongs to protection scope of the present invention.

Claims (9)

1. the method for sodium peroxydisulfate content in a quick mensuration soil, it is characterised in that: comprise the steps:
1) moisture content of soil butt to be measured is measured;
2) according to step 1) in the moisture content that records to calculate the quality of soil butt to be measured be m1, in soil to be measured supplement go from Sub-water, making volume is V1Mud;
3) take the step 2 that volume is V) in mud, add dilute sulfuric acid mixing, stir;
4) to step 3) mixed liquor in add quality be m2Ferrous salt, mix and blend reacts a period of time;
5) by the potassium permanganate solution titration step 4 that concentration is c) in reacted mixed solution, until solution becomes lightpink Till, the potassium permanganate solution volume of consumption is V2
6) sodium peroxydisulfate content in soil butt to be measured is calculated:
2. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 1, it is characterised in that: described step 1) In soil to be measured moisture content use oven drying method measure.
3. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 1, it is characterised in that: described step 2) In pedotheque to be measured be initial soil sample.
4. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 3, it is characterised in that: described step 2) In the mass fraction of mud for preparing be 10~60%.
5. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 4, it is characterised in that: described step 2) In the mass fraction of mud for preparing be 50%.
6. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 1, it is characterised in that: described step 3) The mass fraction of the dilute sulfuric acid of middle addition is 20~40%.
7. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 1, it is characterised in that: described step 4) Middle ferrous salt is ferrous sulfate, ferrous sulfate hydrate, Ferrous ammonium sulfate, Ferrous ammonium sulfate hydrate or ferrous chloride.
8. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 1, it is characterised in that: described step 4) The time of middle mix and blend reaction is 5~15 minutes.
9. the method for sodium peroxydisulfate content in quickly mensuration soil as claimed in claim 1, it is characterised in that: described soil to be measured Earth sample is arranged organizes parallel laboratory test more, and in soil, sodium peroxydisulfate containing measuring the meansigma methods organizing parallel laboratory test more.
CN201610599894.XA 2016-07-27 2016-07-27 A kind of method of sodium peroxydisulfate content in quick measure soil Active CN106053766B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110749695A (en) * 2019-12-04 2020-02-04 上田环境修复有限公司 Method for detecting residual medicament in environmental remediation engineering
CN110749696A (en) * 2019-12-04 2020-02-04 上田环境修复有限公司 Method for detecting residual persulfate in environmental remediation engineering
CN111766334A (en) * 2020-06-09 2020-10-13 天津渤化环境修复股份有限公司 Method for rapidly determining concentration of sodium persulfate in water

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US20070280785A1 (en) * 2004-02-26 2007-12-06 Block Philip A Oxidation Of Organic Compounds At High Ph
CN101576540A (en) * 2009-06-12 2009-11-11 四川大学 Synchronous analysis method of SO4<2->, SO3<2->, S2O6<2-> and S2O8<2-> in pyrolusite leaching solution
US8480903B1 (en) * 2012-11-16 2013-07-09 Jesse Clinton Taylor, III Systems and methods for in-situ contaminant remediation
CN103954614A (en) * 2014-04-21 2014-07-30 复旦大学 Method for rapidly measuring concentration of sodium persulfate in aqueous solution
CN104569288A (en) * 2015-01-21 2015-04-29 北京建工环境修复股份有限公司 Kit and detection method for rapid outdoor detection of residual oxidants in water
CN104624634A (en) * 2015-03-12 2015-05-20 南京科盛环保技术有限公司 Chemical oxidation restoration method for organic polluted soil

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070280785A1 (en) * 2004-02-26 2007-12-06 Block Philip A Oxidation Of Organic Compounds At High Ph
CN101576540A (en) * 2009-06-12 2009-11-11 四川大学 Synchronous analysis method of SO4<2->, SO3<2->, S2O6<2-> and S2O8<2-> in pyrolusite leaching solution
US8480903B1 (en) * 2012-11-16 2013-07-09 Jesse Clinton Taylor, III Systems and methods for in-situ contaminant remediation
CN103954614A (en) * 2014-04-21 2014-07-30 复旦大学 Method for rapidly measuring concentration of sodium persulfate in aqueous solution
CN104569288A (en) * 2015-01-21 2015-04-29 北京建工环境修复股份有限公司 Kit and detection method for rapid outdoor detection of residual oxidants in water
CN104624634A (en) * 2015-03-12 2015-05-20 南京科盛环保技术有限公司 Chemical oxidation restoration method for organic polluted soil

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110749695A (en) * 2019-12-04 2020-02-04 上田环境修复有限公司 Method for detecting residual medicament in environmental remediation engineering
CN110749696A (en) * 2019-12-04 2020-02-04 上田环境修复有限公司 Method for detecting residual persulfate in environmental remediation engineering
CN111766334A (en) * 2020-06-09 2020-10-13 天津渤化环境修复股份有限公司 Method for rapidly determining concentration of sodium persulfate in water

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