CN105823846A - Persulfate oxidation repair analyzing method based on distribution tracer method - Google Patents

Persulfate oxidation repair analyzing method based on distribution tracer method Download PDF

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CN105823846A
CN105823846A CN201610326014.1A CN201610326014A CN105823846A CN 105823846 A CN105823846 A CN 105823846A CN 201610326014 A CN201610326014 A CN 201610326014A CN 105823846 A CN105823846 A CN 105823846A
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tracer
persulfate
aqueous phase
sandbox
concentration
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CN105823846B (en
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翟远征
李木子
滕彦国
王金生
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Beijing Normal University
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography

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Abstract

The invention provides a persulfate oxidation repair analyzing method based on a distribution tracer method .The persulfate oxidation repair analyzing method based on the distribution tracer method comprises the steps that a two-dimensional sand box is established; heavy nonaqueous-phase liquid trichloroethylene is uniformly injected into the two-dimensional sand box, and the saturability and volume of the heavy nonaqueous-phase liquid are measured with the volume distribution tracer method; an ion chromatograph is used for measuring the concentration of a conservative tracer Br-, and a gas chromatograph is used for measuring the concentration of trichloroethylene and the concentration of alcohol of a volume distribution tracer; the oxidation repair effect of persulfate is analyzed according to the saturability and volume changing conditions of the heavy nonaqueous-phase liquid and the concentration changing conditions of trichloroethylene in liquid flowing out of the sand box at different moments .By establishing the two-dimensional sand box, the saturability and volume of the heavy nonaqueous-phase liquid and the concentration of trichloroethylene in flowing out liquid are measured with the distribution tracer method so that the oxidation repair effect of persulfate can be accurately analyzed, and a reference can be provided for in-situ repair of heavy nonaqueous-phase liquid .

Description

A kind of persulfate oxidation repairing analysis method based on distribution tracer method
Technical field
The present invention relates to Organic Contamination of Groundwater technical field, particularly relate to a kind of mistake based on distribution tracer method Oxide sulfate repairing analysis method.
Background technology
In recent years, Organic Contamination of Groundwater has become the current protection of groundwater environment in the world and the focus administered Problem.The oxidation repairing effect of persulfate cannot be analyzed by groundwater remediation technology accurately.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of persulfate oxidation based on distribution tracer method and repaiies Complex analytic method, it is possible to the oxidation reparation to persulfate accurately is analyzed.
For solving above-mentioned technical problem, embodiments of the invention provide a kind of persulfuric acid based on distribution tracer method Salt oxidation repairing analysis method, described persulfate oxidation repairing analysis method bag based on distribution tracer method Include:
Set up two dimension sandbox；
In described two dimension sandbox, inject dense non-aqueous phase liquids trichloro ethylene uniformly, utilize capacity distribution spike Method is for measuring saturation and the volume of dense non-aqueous phase liquids；
Use ion chromatograph that conservative tracer Br-concentration is measured, use gas chromatograph for determination three Vinyl chloride and alcohols capacity distribution tracer alcohol concentration；
Saturation according to dense non-aqueous phase liquids the most in the same time and change in volume situation and trichloro ethylene concentration become Change situation analysis and cross the oxidation repairing effect of persulfate.
Preferably, described foundation two dimension sandbox, including:
Protecting glass for steel before foundation, other faces are the two-dimentional sandbox of corrosion resistant plate, in described two dimension sandbox Uniformly filled natural quartz sand；
Solution inlet is set at two dimension sandbox left side wall, pollutant inlet is set at two dimension sandbox roof, At two dimension sandbox right side wall, solution flow export is set；
Efficient liquid-phase chromatographic pump is used to be injected in two dimension sandbox by solution inlet by reactor solution.
Preferably, described uniform filled natural quartz sand in described two dimension sandbox, including:
Ultra-pure water after using funnel the sand after clean drying and degassing to be processed alternately is slowly added to, and fills out by several times Fill, equal disturbance compacting before each back-up sand；
With ultra-pure water, device is carried out drip washing, remove the impurity introduced in filling process.
Preferably, described injection dense non-aqueous phase liquids trichloro ethylene in described two dimension sandbox uniformly, including:
Syringe is used to be injected by the pollutant inlet of two dimension sandbox by trichloro ethylene.
Preferably, trichloro ethylene is injected by described use syringe by the pollutant inlet of two dimension sandbox, bag Include:
Syringe needle insertion depth is distance sandbox top 9cm, forms some injection source, and charge velocity is 0.2mL/min；
After injection terminates, device is stood and within 48 hours, makes trichloro ethylene the most naturally migrate.
Preferably, described utilize capacity distribution tracer method for measuring saturation and the body of dense non-aqueous phase liquids Long-pending, including:
Utilize following formula measure dense non-aqueous phase liquids saturation:
R p t = μ r μ c = 1 + ρ b K d θ w + K n w S n 1 - S n
Wherein, SnSaturation R for dense non-aqueous phase liquidsptFor the retardation coefficient of capacity distribution tracer, by μr And μcRatio be worth to；μrAnd μcRefer to capacity distribution tracer and the retention time of conservative tracer, K respectivelynw For the partition coefficient between nonaqueous phase and aqueous phase, KdFor tracer partition coefficient in aqueous phase and solid phase；
Utilize following formula:
V N = P V S n 1 - S n
Wherein, VNFor the volume of dense non-aqueous phase liquids, PV is pore volume.
Preferably, the described saturation utilizing following formula to measure dense non-aqueous phase liquids, including:
Work as KdValue 0, KnwDuring value 38.2, μ is calculated:
μ = ∫ 0 ∞ t C d t ∫ 0 ∞ C d t -0 .5 ∫ 0 ∞ C d t
Wherein, C is corresponding tracer concentration the most in the same time, and t is the migration time of tracer.
Preferably, described utilize capacity distribution tracer method for measuring saturation and the body of dense non-aqueous phase liquids Long-pending, including:
In sandbox, inject persulfate carry out in-situ oxidation, change dense non-aqueous phase liquids saturation；
According to the amount of injection persulfate, being divided into five groups of injections, corresponding persulfate PV number is followed successively by 0, 3,6,9,12；
Often group is injected and is first injected Br-, reinject alcohols；
After carrying out 4 PV, inject liquid and switched to saturated trichloro ethylene solution to carry out drip washing by reactor solution, Until effluent tracer relative concentration reduces to zero.
Preferably, conservative tracer Br-concentration is measured by described use ion chromatograph, uses gas phase Chromatograph measures trichloro ethylene and capacity distribution tracer alcohol concentration, including:
Use ion chromatograph to Br-Concentration is measured；
Use gas chromatograph for determination trichloro ethylene and alcohol concentration；
Heating schedule is: gas chromatograph tubing string initial temperature is set to 45 DEG C and lasting 3min, afterwards 160 degrees Celsius are risen to the speed of 10 degrees Celsius per minute.
Preferably, the saturation of described basis dense non-aqueous phase liquids the most in the same time and change in volume situation and trichlorine Ethylene concentration situation of change analyzed the oxidation repairing effect of persulfate, including:
When saturation, volume and the trichloro ethylene concentration of dense non-aqueous phase liquids is along with injecting persulfate PV number Increase when constantly reducing, show that the oxidation repairing effect of persulfate is obvious.
Having the beneficial effect that of the technique scheme of the present invention:
In such scheme, by setting up two dimension sandbox, distribution tracer method is used to measure dense non-aqueous phase liquids saturated Trichloro ethylene concentration in degree, dense non-aqueous phase liquids volume and effluent, it is possible to analyze persulfate accurately Oxidation repairing effect, the in-situ immobilization for dense non-aqueous phase liquids provides reference.
Accompanying drawing explanation
Fig. 1 is the persulfate oxidation repairing analysis method stream based on distribution tracer method of the embodiment of the present invention Cheng Tu.
Detailed description of the invention
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with attached Figure and specific embodiment are described in detail.
As it is shown in figure 1, a kind of persulfate oxidation reparation based on distribution tracer method of embodiments of the invention divides Analysis method, described persulfate oxidation repairing analysis method based on distribution tracer method includes:
Step 101: set up two dimension sandbox.
Step 102: inject dense non-aqueous phase liquids trichloro ethylene in described two dimension sandbox uniformly, utilize body Integration joins tracer method for measuring saturation and the volume of dense non-aqueous phase liquids.
Step 103: use ion chromatograph that conservative tracer Br-concentration is measured, use gas phase color Spectrometer measures trichloro ethylene and capacity distribution tracer alcohol concentration.
Step 104: according to the saturation of dense non-aqueous phase liquids the most in the same time and change in volume situation and three chloroethenes The oxidation repairing effect of persulfate is crossed in alkene concentration change situation analysis.
The persulfate oxidation repairing analysis method based on distribution tracer method of the embodiment of the present invention, by setting up Two dimension sandbox, uses distribution tracer method to measure dense non-aqueous phase liquids saturation, dense non-aqueous phase liquids volume and stream Go out trichloro ethylene concentration in liquid, it is possible to analyze the oxidation repairing effect of persulfate, nonaqueous phase of attaching most importance to accurately The in-situ immobilization of liquid provides reference.
Preferably, described foundation two dimension sandbox, including:
Protecting glass for steel before foundation, other faces are the two-dimentional sandbox of corrosion resistant plate, in described two dimension sandbox Uniformly filled natural quartz sand；
Solution main-inlet is set at two dimension sandbox left side wall, pollutant inlet is set at two dimension sandbox roof, At two dimension sandbox right side wall, solution flow export is set；
Efficient liquid-phase chromatographic pump is used to be injected in two dimension sandbox by solution inlet by reactor solution.
Wherein, two dimension sandbox left side wall is evenly arranged with three solution inlets, and two dimension sandbox roof uniformly sets Being equipped with five pollutant inlets, two dimension sandbox right side wall is evenly arranged with three solution flow exports.
Preferably, described uniform filled natural quartz sand in described two dimension sandbox, including:
Ultra-pure water after using funnel the sand after clean drying and degassing to be processed alternately is slowly added to, and fills out by several times Fill, equal disturbance compacting before each back-up sand；
With ultra-pure water, device is carried out drip washing, remove the impurity introduced in filling process.
Wherein it is possible to the filled media used is the good natural siliceous sand of sorting, the type of sand is 40/50, median particle size is 0.36mm.Choose trichloro ethylene as typical case's dense non-aqueous phase liquids.For ease of seeing Examine migration path and the distribution of trichloro ethylene, use 100mg L-1Sudan IV (Aldrich) It is dyeed.Use 100mg L-1Alcohols as capacity distribution tracer, its breakthrough curve is used for surveying Determine dense non-aqueous phase liquids saturation；200mg·L-1Bromine as conservative tracer, the migration of this tracer is not Adsorbed by medium and dense non-aqueous phase liquids and affected, can be as the reduced value of capacity distribution tracer flow.Use The sodium peroxydisulfate of 5mmol/L and the persulfate of the ferrous sulfate preparation ferrous ion catalysis of 0.8mmol/L As in situ chemical oxidation agent.
Preferably, described injected slurry volume distribution tracer trichloro ethylene, bag in described two dimension sandbox uniformly Include:
Syringe is used to be injected by the pollutant inlet of two dimension sandbox by trichloro ethylene.
Preferably, trichloro ethylene is injected by described use syringe by the pollutant inlet of two dimension sandbox, bag Include:
Syringe needle insertion depth is distance sandbox top 9cm, forms some injection source, and charge velocity is 0.2mL/min；
After injection terminates, device is stood and within 48 hours, makes trichloro ethylene the most naturally migrate.
Preferably, described utilize capacity distribution tracer method for measuring saturation and the body of dense non-aqueous phase liquids Long-pending, including:
Utilize following formula measure dense non-aqueous phase liquids saturation:
R p t = μ r μ c = 1 + ρ b K d θ w + K n w S n 1 - S n
Wherein, SnSaturation R for dense non-aqueous phase liquidsptFor the retardation coefficient of capacity distribution tracer, by μr And μcRatio be worth to；μrAnd μcRefer to capacity distribution tracer and the retention time of conservative tracer, K respectivelynw For the partition coefficient between nonaqueous phase and aqueous phase, KdFor tracer partition coefficient in aqueous phase and solid phase；
Utilize following formula:
V N = P V S n 1 - S n
Wherein, VNFor the volume of dense non-aqueous phase liquids, PV is pore volume.
Preferably, the described saturation utilizing following formula to measure dense non-aqueous phase liquids, including:
Work as KdValue 0, KnwDuring value 38.2, μ is calculated:
μ = ∫ 0 ∞ t C d t ∫ 0 ∞ C d t - 0.5 ∫ 0 ∞ C d t
Wherein, C is corresponding tracer concentration the most in the same time, and t is the migration time of tracer.
Preferably, described utilize capacity distribution tracer method for measuring saturation and the body of dense non-aqueous phase liquids Long-pending, including:
In sandbox, inject persulfate carry out in-situ oxidation, change dense non-aqueous phase liquids saturation；
According to the amount of injection persulfate, being divided into five groups of injections, corresponding persulfate PV number is followed successively by 0, 3,6,9,12；
Often group is injected and is first injected Br-, reinject alcohols；
After carrying out 4 PV, inject liquid and switched to saturated trichloro ethylene solution to carry out drip washing by reactor solution, Until effluent tracer relative concentration reduces to zero.
Preferably, conservative tracer Br-concentration is measured by described use ion chromatograph, uses gas phase Chromatograph measures trichloro ethylene and capacity distribution tracer alcohol concentration, including:
Use ion chromatograph to Br-Concentration is measured；
Use gas chromatograph for determination trichloro ethylene and alcohol concentration；
Heating schedule is: gas chromatograph tubing string initial temperature is set to 45 DEG C and lasting 3min, afterwards 160 degrees Celsius are risen to the speed of 10 degrees Celsius per minute.
Wherein, in order to analyze the change of trichloro ethylene concentration in persulfate oxidation degradation process, to effluent Middle trichloro ethylene concentration carries out METHOD FOR CONTINUOUS DETERMINATION, until dense non-aqueous phase liquids is degradable.Use glass syringe Sampling, frequency is 1 time/PV (PV refers to the persulfate PV number injected), measures three chloroethenes after sampling immediately Alkene concentration.
Preferably, the saturation of described basis dense non-aqueous phase liquids the most in the same time and change in volume situation and trichlorine Ethylene concentration situation of change analyzed the oxidation repairing effect of persulfate, including:
When saturation, volume and the trichloro ethylene concentration of dense non-aqueous phase liquids is along with injecting persulfate PV number Increase when constantly reducing, show that the oxidation repairing effect of persulfate is obvious.
In such scheme, by setting up two dimension sandbox, distribution tracer method is used to measure dense non-aqueous phase liquids saturated Trichloro ethylene concentration in degree, dense non-aqueous phase liquids volume and effluent, it is possible to analyze persulfate accurately Oxidation repairing effect, the in-situ immobilization for dense non-aqueous phase liquids provides reference.
The above is the preferred embodiment of the present invention, it is noted that for the common skill of the art For art personnel, on the premise of without departing from principle of the present invention, it is also possible to make some improvements and modifications, These improvements and modifications also should be regarded as protection scope of the present invention.

Claims (10)

1. a persulfate oxidation repairing analysis method based on distribution tracer method, it is characterised in that institute State persulfate oxidation repairing analysis method based on distribution tracer method to include:
Set up two dimension sandbox；
In described two dimension sandbox, inject dense non-aqueous phase liquids trichloro ethylene equably, utilize capacity distribution spike Method is for measuring saturation and the volume of dense non-aqueous phase liquids；
Use ion chromatograph that conservative tracer Br-concentration is measured, use gas chromatograph for determination three Vinyl chloride and capacity distribution tracer alcohol concentration；
In saturation according to dense non-aqueous phase liquids the most in the same time and change in volume situation and sandbox effluent three The oxidation repairing effect of persulfate is crossed in vinyl chloride concentration change situation analysis.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 1, It is characterized in that, described foundation two dimension sandbox, including:
Protecting glass for steel before foundation, other faces are the two-dimentional sandbox of corrosion resistant plate, in described two dimension sandbox Uniformly filled natural quartz sand；
Solution inlet is set at two dimension sandbox left side wall, pollutant inlet is set at two dimension sandbox roof, At two dimension sandbox right side wall, solution flow export is set；
Efficient liquid-phase chromatographic pump is used to be injected in two dimension sandbox by solution inlet by reactor solution.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 2, It is characterized in that, described uniform filled natural quartz sand in described two dimension sandbox, including:
Ultra-pure water after using funnel the sand after clean drying and degassing to be processed alternately is slowly added to, and fills out by several times Fill, equal disturbance compacting before each back-up sand；
With ultra-pure water, device is carried out drip washing, remove the impurity introduced in filling process.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 1, It is characterized in that, described injection dense non-aqueous phase liquids trichloro ethylene in described two dimension sandbox uniformly, including:
Syringe is used to be injected by the pollutant inlet of two dimension sandbox by trichloro ethylene.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 4, It is characterized in that, trichloro ethylene is injected by described use syringe by the pollutant inlet of two dimension sandbox, bag Include:
Syringe needle insertion depth is distance sandbox top 9cm, forms some injection source, and charge velocity is 0.2mL/min；
After injection terminates, device is stood and within 48 hours, makes trichloro ethylene the most naturally migrate.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 1, It is characterized in that, described utilize capacity distribution tracer method for measuring saturation and the body of dense non-aqueous phase liquids Long-pending, including:
Utilize following formula measure dense non-aqueous phase liquids saturation:
R p t = μ r μ c = 1 + ρ b K d θ w + K n w S n 1 - S n
Wherein, SnSaturation R for dense non-aqueous phase liquidsptFor the retardation coefficient of capacity distribution tracer, by μr And μcRatio be worth to；μrAnd μcRefer to capacity distribution tracer and the retention time of conservative tracer, K respectivelynw For the partition coefficient between nonaqueous phase and aqueous phase, KdFor tracer partition coefficient in aqueous phase and solid phase；
Utilize following formula:
V N = P V S n 1 - S n
Wherein, VNFor the volume of dense non-aqueous phase liquids, PV is pore volume.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 6, It is characterized in that, the described saturation utilizing following formula to measure dense non-aqueous phase liquids, including:
Work as KdValue 0, KnwDuring value 38.2, μ is calculated:
μ = ∫ 0 ∞ t C d t ∫ 0 ∞ C d t - 0.5 ∫ 0 ∞ C d t
Wherein, C is corresponding tracer concentration the most in the same time, and t is the migration time of tracer.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 1, It is characterized in that, described utilize capacity distribution tracer method for measuring saturation and the body of dense non-aqueous phase liquids Long-pending, including:
In sandbox, inject persulfate carry out in-situ oxidation, change dense non-aqueous phase liquids saturation；
According to the amount of injection persulfate, being divided into five groups of injections, corresponding persulfate PV number is followed successively by 0, 3,6,9,12；
Often group is injected and is first injected Br-, reinject alcohols；
After carrying out 4 PV, inject liquid and switched to saturated trichloro ethylene solution to carry out drip washing by reactor solution, Until effluent tracer relative concentration reduces to zero.
Persulfate oxidation repairing analysis method based on distribution tracer method the most according to claim 1, It is characterized in that, conservative tracer Br-concentration is measured by described use ion chromatograph, uses gas phase Chromatograph measures trichloro ethylene and capacity distribution tracer alcohol concentration, including:
Use ion chromatograph to Br-Concentration is measured；
Use gas chromatograph for determination trichloro ethylene and alcohol concentration；
Heating schedule is: gas chromatograph tubing string initial temperature is set to 45 DEG C and lasting 3min, afterwards 160 degrees Celsius are risen to the speed of 10 degrees Celsius per minute.
Persulfate oxidation repairing analysis side based on distribution tracer method the most according to claim 1 Method, it is characterised in that the saturation of described basis dense non-aqueous phase liquids the most in the same time and change in volume situation and The oxidation repairing effect of persulfate is crossed in trichloro ethylene concentration change situation analysis, including:
When in saturation, volume and the sandbox effluent of dense non-aqueous phase liquids trichloro ethylene concentration along with injecting When the increase of sulfate PV number constantly reduces, show that the oxidation repairing effect of persulfate is obvious.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112485835A (en) * 2020-10-28 2021-03-12 南京大学 Method for finely depicting heavy non-aqueous phase polluted site by fusing multi-source observation data
CN112485835B (en) * 2020-10-28 2021-09-28 南京大学 Method for finely depicting heavy non-aqueous phase polluted site by fusing multi-source observation data

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