CN112444513B - Polycyclic aromatic hydrocarbon contaminated soil restoration effect evaluation method and detection kit - Google Patents
Polycyclic aromatic hydrocarbon contaminated soil restoration effect evaluation method and detection kit Download PDFInfo
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Abstract
The invention provides a method for detecting polycyclic aromatic hydrocarbon pollutants in soil, which comprises the following steps of S1, adding an extractant into a soil sample, concentrating and fixing the volume to obtain a sample solution to be detected; s2, adding the sample solution to be detected into a mixed solution of formaldehyde and concentrated sulfuric acid, observing a reaction result, and comparing the reaction result with the reaction result of polycyclic aromatic hydrocarbon standard substance solutions with different concentrations and the mixed solution of formaldehyde and concentrated sulfuric acid to obtain the concentration of polycyclic aromatic hydrocarbon in soil.
Description
Technical Field
The invention relates to the technical field of soil organic pollutant detection, in particular to a polycyclic aromatic hydrocarbon polluted soil restoration effect evaluation method and a detection kit.
Background
With the promotion of the industrialization process of China and the implementation of the urban development strategy of China 'two-in-three', the problem of pollution sites is increasingly remarkable, and pollution sites and soil pollution and public nuisance incidents caused by enterprises such as petroleum, chemical industry, smelting, mine and the like frequently occur. Polycyclic Aromatic Hydrocarbons (PAHs) are one of common pollutants in organic pollution sites such as petroleum, chemical industry and the like, have the effects of carcinogenesis, teratogenesis and mutagenesis, are easy to adsorb in soil particles for a long time, and therefore become one of the indexes of great concern in site investigation and repair processes. The land screening value of PAHs substances is definitely regulated in GB 36600-2018 land pollution risk management and control standard (trial) for soil environmental quality construction, wherein the minimum concentration screening value of benzo [ a ] pyrene and other substances is 0.55mg/kg.
The remediation technology of the polycyclic aromatic hydrocarbon contaminated soil mainly comprises thermal desorption, chemical oxidation and the like, and the remediation effect of the technology is generally judged by measuring the concentration of polycyclic aromatic hydrocarbon substances in the soil: the collected soil sample is sent to a related detection laboratory, and after being treated by extraction, purification, concentration and the like in the laboratory, the soil sample is analyzed and measured by a large-scale instrument such as a gas chromatograph-mass spectrometer or a high performance liquid chromatograph. The method has the advantages of high detection precision, complex operation, long time consumption and high cost, can not timely and rapidly detect the concentration level of the polycyclic aromatic hydrocarbon pollutants on the site of the engineering project, and can not timely reflect the treatment effect of the repair technology or process on the polycyclic aromatic hydrocarbon pollutants.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that the detection method of the polycyclic aromatic hydrocarbon polluted soil in the prior art is complex in operation, long in time consumption and high in cost, and the polycyclic aromatic hydrocarbon restoration effect cannot be timely and rapidly reflected on site, and provide the detection method and the kit which are simple in operation, short in time consumption and low in cost, and can timely and rapidly reflect the polycyclic aromatic hydrocarbon concentration and the restoration effect on site.
Therefore, the invention provides a method for detecting polycyclic aromatic hydrocarbon pollutants in soil, which comprises the following steps of,
s1, adding an extractant into a soil sample, concentrating and fixing the volume to obtain a sample solution to be detected;
s2, mixing the sample solution to be detected with a mixed solution of formaldehyde and concentrated sulfuric acid, observing a reaction result, and comparing the reaction result with the reaction result of the polycyclic aromatic hydrocarbon standard substance solution with different concentrations and the mixed solution of formaldehyde and concentrated sulfuric acid to obtain the concentration of the polycyclic aromatic hydrocarbon in the soil.
In the method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil, in the step S1, the extractant is one or two of normal hexane and methylene dichloride; the volume is determined by adding the extractant according to the ratio of the mass (g) of the soil sample to the volume (mL) =1:1 of the extract.
In the method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil, in the step S1, the ratio of the extractant to the soil sample is 30:1 (volume (mL): mass (g)), and the extraction is performed for at least 3 times by shaking.
In the S2 step, the mixed solution of formaldehyde and concentrated sulfuric acid is obtained by mixing formaldehyde solution and concentrated sulfuric acid according to the volume ratio of 1:9-1:1000; the mass fraction of the formaldehyde solution is 37%, and the mass fraction of the concentrated sulfuric acid is 98.3%.
In the method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil, in the step S2, the polycyclic aromatic hydrocarbon in the polycyclic aromatic hydrocarbon standard substance solution is naphthalene, acenaphthylene dihydro, fluorene, phenanthrene, anthracene, fluoranthene, pyrene and benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzeneAnd [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]Perylene.
According to the detection method of the polycyclic aromatic hydrocarbon pollutants in the soil, the concentrations of the polycyclic aromatic hydrocarbon standard substance solutions are respectively 0.25 mug/mL, 0.5 mug/mL, 1 mug/mL, 5 mug/mL, 10 mug/mL and 50 mug/mL.
In the method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil, in the step S2, each 0.1mL of the sample solution to be detected is mixed with 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid; each 0.1mL of the polycyclic aromatic hydrocarbon standard solution is mixed with 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid.
The method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil further comprises the steps of drying, grinding and sieving the soil sample by a 20-mesh sieve before adding the extractant into the soil sample.
The method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil comprises the steps of drying in the air, air drying, freeze drying, adding calcium oxide or adding one or more of anhydrous sodium sulfate.
The method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil further comprises the step of adding a strong alkali solution after detection is completed, wherein the strong alkali is one or two of sodium hydroxide and potassium hydroxide.
The invention also provides a kit for detecting the polycyclic aromatic hydrocarbon, which comprises a box body, a cover body arranged on the box body and also comprises,
the reaction disc is provided with reaction holes, and the reaction Kong Nacheng is used for placing the mixed solution of formaldehyde and concentrated sulfuric acid;
polycyclic aromatic hydrocarbon sample bottle, hold polycyclic aromatic hydrocarbon standard substance solution of different concentration in the polycyclic aromatic hydrocarbon sample bottle.
The kit for detecting the polycyclic aromatic hydrocarbon also comprises a strong alkali sample bottle, a liquid-transferring gun, a gun head matched with the liquid-transferring gun and gloves; wherein, hold strong base solid in the strong base sample bottle.
The kit for detecting the polycyclic aromatic hydrocarbon is characterized in that 10-96 reaction holes are formed in the reaction disc; each of the reactions Kong Nacheng was placed with 0.9mL of a mixed solution of formaldehyde and concentrated sulfuric acid.
The kit for detecting the polycyclic aromatic hydrocarbon comprises 6 polycyclic aromatic hydrocarbon sample bottles, namely a first polycyclic aromatic hydrocarbon sample bottle, a second polycyclic aromatic hydrocarbon sample bottle, a third polycyclic aromatic hydrocarbon sample bottle, a fourth polycyclic aromatic hydrocarbon sample bottle, a fifth polycyclic aromatic hydrocarbon sample bottle and a sixth polycyclic aromatic hydrocarbon sample bottle, wherein the concentration of the contained polycyclic aromatic hydrocarbon standard substance solution is 0.25 mug/mL, 0.5 mug/mL, 1 mug/mL, 5 mug/mL, 10 mug/mL and 50 mug/mL respectively.
The volume of the polycyclic aromatic hydrocarbon sample bottle is 2mL, and each polycyclic aromatic hydrocarbon sample bottle contains 1mL of polycyclic aromatic hydrocarbon standard substance solution.
The volume of the strong base sample bottle is 60mL, and 100g of strong base solid is contained in the strong base sample bottle; the measuring range of the pipette is 200 mu L; the number of gun heads matched with the pipetting gun is 100; the glove is specifically a pair of latex gloves 2.
The kit for detecting the polycyclic aromatic hydrocarbon comprises a liner with a groove, wherein the liner is used for fixing the reaction disc, the polycyclic aromatic hydrocarbon sample bottle, the strong alkali sample bottle, the pipette gun, a gun head matched with the pipette gun and gloves.
The technical scheme of the invention has the following advantages:
1. the invention provides a method for detecting polycyclic aromatic hydrocarbon pollutants in soil, which comprises the following steps of S1, adding an extractant into a soil sample, concentrating and fixing the volume to obtain a sample solution to be detected; s2, mixing the sample solution to be detected with a mixed solution of formaldehyde and concentrated sulfuric acid, observing a reaction result, comparing the reaction result with a reaction result of a polycyclic aromatic hydrocarbon standard substance solution with different concentrations and the mixed solution of formaldehyde and concentrated sulfuric acid to obtain the concentration of polycyclic aromatic hydrocarbon in soil, wherein the polycyclic aromatic hydrocarbon and formaldehyde can generate a dark green polymer under the action of the concentrated sulfuric acid, the polymer is insoluble in a sulfuric acid-n-hexane or sulfuric acid-dichloromethane system, can be directly observed by naked eyes, and the polycyclic aromatic hydrocarbon in the soil can be fully extracted by adding an extracting agent; by utilizing the principle, the method is used for detecting the polycyclic aromatic hydrocarbon concentration of the soil, has the advantages of simple operation, short time consumption and low cost, can complete detection on a soil restoration site without sending the sample into a laboratory, and timely and rapidly reflects the restoration effect of the polycyclic aromatic hydrocarbon.
2. In the S1 step, the extractant is one or two of n-hexane and dichloromethane; the constant volume is that the extractant is added according to the mass (g) of the soil sample, namely the ratio of the volume (mL) =1:1, so as to carry out constant volume, and one or two of normal hexane and methylene dichloride are adopted as the extractant, so that on one hand, polycyclic aromatic hydrocarbon can be extracted better, and on the other hand, the production of dark green polymer can be ensured; the concentration of the polycyclic aromatic hydrocarbon in the soil can be accurately estimated by carrying out volume fixing according to the ratio of the mass (g) of the soil sample to the volume (mL) =1:1 of the extract.
3. In the S2 step, the mixed solution of formaldehyde and concentrated sulfuric acid is obtained by mixing formaldehyde solution and concentrated sulfuric acid according to the volume ratio of 1:9-1:1000; the formaldehyde solution is 37% in mass fraction, the concentrated sulfuric acid is 98.3% in mass fraction, formaldehyde and polycyclic aromatic hydrocarbon dissolved in normal hexane or methylene dichloride can be reacted under the action of the concentrated sulfuric acid by mixing the formaldehyde solution and the concentrated sulfuric acid in the volume ratio of 1:9-1:1000, so that the dark green polymer is obtained, the concentration level of the polycyclic aromatic hydrocarbon can be estimated directly through visual inspection due to the fact that the polymer is not dissolved in a sulfuric acid-normal hexane or sulfuric acid-methylene dichloride system, the operation is simple, the time consumption is short, the cost is low, the detection can be completed on a soil restoration site without sending a sample into a laboratory, and the restoration effect of the polycyclic aromatic hydrocarbon can be timely and rapidly reflected.
4. According to the detection method for the polycyclic aromatic hydrocarbon pollutants in the soil, the concentration of the polycyclic aromatic hydrocarbon standard substance solution is 0.25 mug/mL, 0.5 mug/mL, 1 mug/mL, 5 mug/mL, 10 mug/mL and 50 mug/mL respectively, when the concentration of the polycyclic aromatic hydrocarbon is lower than 0.5 mug/mL, the black-free green polymer is generated, when the concentration is higher than 0.5 mug/mL, the black-green polymer can be generated, and as the concentration is increased, the amount of the polymer is gradually increased, and as the minimum screening value of the polycyclic aromatic hydrocarbon in the first type construction land soil pollution risk management standard (test) is regulated in GB 36600-2018, the method can be used for evaluating whether the polycyclic aromatic hydrocarbon substances reach the standard in the repair treatment process, namely, when no sediment is generated, the polycyclic aromatic hydrocarbon concentration in the soil reaches the standard; when sediment is generated, the concentration of the polycyclic aromatic hydrocarbon in the soil does not reach the standard; and the concentration of the polycyclic aromatic hydrocarbon standard substance solution is set to be 0.25 mug/mL, 0.5 mug/mL, 1 mug/mL, 5 mug/mL, 10 mug/mL and 50 mug/mL, the concentration of the polycyclic aromatic hydrocarbon in the sample to be detected can be estimated approximately by comparing the amount of the polymer generated by the sample to be detected with the amounts of the polymers generated by the polycyclic aromatic hydrocarbon standard substance solutions with different concentrations, the operation is simple, the time consumption is short, the cost is low, the sample is not required to be sent into a laboratory, the detection can be completed on the soil restoration site, and the restoration effect of the polycyclic aromatic hydrocarbon can be reflected timely and rapidly.
5. In the S2 step, each 0.1mL of the sample solution to be detected is mixed with 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid; every 0.1mL of the polycyclic aromatic hydrocarbon standard solution is mixed with 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid, and the smooth progress of the reaction can be ensured by limiting the proportion of the sample solution to be detected, the polycyclic aromatic hydrocarbon standard solution and the mixed solution of formaldehyde and concentrated sulfuric acid, and the concentration of polycyclic aromatic hydrocarbon in the sample to be detected can be conveniently estimated.
6. According to the method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil, the steps of drying, grinding and sieving with a 20-mesh sieve are further included before the extractant is added into the soil sample, and the soil sample is dried, ground and sieved to prepare for subsequent extraction, so that polycyclic aromatic hydrocarbons can be extracted from the soil more conveniently.
7. The method for detecting the polycyclic aromatic hydrocarbon pollutants in the soil provided by the invention further comprises the step of adding a strong alkali solution after detection is completed, wherein the strong alkali is one or two of sodium hydroxide and potassium hydroxide, and the concentrated sulfuric acid is involved in the detection process, so that the concentrated sulfuric acid can be neutralized by adding the strong alkali solution after detection is completed, and environment friendliness is realized.
8. The invention provides a kit for detecting polycyclic aromatic hydrocarbon, which comprises a box body and a cover body arranged on the box body, and further comprises: the reaction disc is provided with reaction holes, and the reaction Kong Nacheng is used for placing the mixed solution of formaldehyde and concentrated sulfuric acid; polycyclic aromatic hydrocarbon sample bottle, hold polycyclic aromatic hydrocarbon standard substance solution of different concentration in the polycyclic aromatic hydrocarbon sample bottle. The polycyclic aromatic hydrocarbon and formaldehyde can generate a dark green polymer under the action of concentrated sulfuric acid, and the polymer is insoluble in a sulfuric acid-n-hexane or sulfuric acid-dichloromethane system and can be directly observed by a visual method; by utilizing the principle, by arranging the reaction plate and adding the mixed solution of formaldehyde and concentrated sulfuric acid into the reaction holes of the reaction plate, a sample solution to be detected, which is obtained by extraction with normal hexane or dichloromethane, can be added into the mixed solution, and whether dark green polymers are generated or not is observed; meanwhile, polycyclic aromatic hydrocarbon standard substance solutions with different concentrations are added into the reaction holes, and the dark green polymer generated by the sample solution to be detected is compared with the dark green polymer generated by the standard substance solution, so that the concentration of polycyclic aromatic hydrocarbon in the sample to be detected is estimated. Through setting up the polycyclic aromatic hydrocarbon sample bottle that holds polycyclic aromatic hydrocarbon standard substance solution, can provide the reference standard for polycyclic aromatic hydrocarbon's concentration detection, adopt this kit to carry out the polycyclic aromatic hydrocarbon concentration detection of soil, easy operation, consuming time are short, with low costs, need not send the sample into the laboratory, can accomplish the detection at soil repair scene, in time, reflect polycyclic aromatic hydrocarbon's restoration effect fast.
9. The invention provides a kit for detecting polycyclic aromatic hydrocarbon, which also comprises a strong alkali sample bottle, a liquid-transferring gun, a gun head matched with the liquid-transferring gun and a glove; the strong alkali sample bottle contains strong alkali solid, and the reaction hole contains concentrated sulfuric acid, so that strong alkali can be added into the reaction hole to neutralize acidity after detection is finished by arranging the strong alkali sample bottle, thereby preventing pollution to the environment and realizing environmental friendliness; by arranging the liquid-transferring gun and the gun head, the sample can be conveniently sucked and transferred; through setting up gloves, can protect operating personnel, improve the security of operation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of a kit for detection of polycyclic aromatic hydrocarbons according to examples 2 to 3 of the present invention;
1-a reaction plate; 2-reaction wells; 3-a pad; 4-a strong base sample bottle; 5-a pipette; 6-gun head; 7-gloves; 8-a box body; 9-a cover; 10-a first polycyclic aromatic hydrocarbon sample bottle; 11-a second polycyclic aromatic hydrocarbon sample bottle; 12-a third polycyclic aromatic hydrocarbon sample bottle; 13-fourth polycyclic aromatic hydrocarbon sample bottle; 14-a fifth polycyclic aromatic hydrocarbon sample bottle; 15-sixth polycyclic aromatic hydrocarbon sample bottle.
Detailed Description
Example 1
The embodiment provides a method for detecting polycyclic aromatic hydrocarbon pollutants in soil, which comprises the following steps,
s1, taking a soil sample, airing, grinding, sieving with a 20-target standard sieve to obtain a ground soil sample, taking 0.1g of the ground soil sample into a 10mL glass centrifuge tube, adding 3mL of n-hexane into the ground soil sample, vibrating for 5min for extraction, centrifuging at 2000rpm for 5min, transferring the supernatant into a clean glass centrifuge tube with scales by using a suction tube, repeating the steps for three times, merging the supernatant, putting the centrifuge tube containing an extract into water at 40 ℃, heating and concentrating, and then fixing the volume to 0.1mL by using n-hexane to obtain a sample solution to be detected.
S2, mixing a formaldehyde solution with the mass fraction of 37% with concentrated sulfuric acid with the mass fraction of 98.3% according to the volume ratio of 1:9 to obtain a mixed solution of formaldehyde and concentrated sulfuric acid; adding 0.1mL of the sample solution to be detected obtained in the step S1 into 0.9mL of a mixed solution of formaldehyde and concentrated sulfuric acid, observing whether dark green polymers are generated, if no dark green polymers are generated, indicating that the amount of polycyclic aromatic hydrocarbon in the soil sample is lower than 0.5mg/kg, and if the dark green polymers are generated, respectively taking 0.25 mug/mL, 0.5 mug/mL, 1 mug/mL, 5 mug/mL, 10 mug/mL and 50 mug/mL of polycyclic aromatic hydrocarbon standard substance solution, wherein 0.1mL of polycyclic aromatic hydrocarbon standard substance solution is added into 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid, and the polycyclic aromatic hydrocarbon standard substance solution is naphthalene, acenaphthylene, dihydro acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]And (3) the amount of the dark green polymer generated by the sample solution to be detected is compared with the amount of the dark green polymer generated by the polycyclic aromatic hydrocarbon standard solution with 6 concentrations, so that the approximate concentration of the polycyclic aromatic hydrocarbon in the soil is determined.
The embodiment also provides a kit for detecting polycyclic aromatic hydrocarbon, which comprises a box body 8 and a cover body 9 arranged on the box body 8, and further comprises a reaction plate 1 and a polycyclic aromatic hydrocarbon sample bottle, wherein 96 reaction holes 2 are formed in the reaction plate 1, mixed solution of formaldehyde and concentrated sulfuric acid is contained in the reaction holes 2, wherein the mixed solution of formaldehyde and concentrated sulfuric acid is obtained by mixing formaldehyde solution with the mass fraction of 37% with concentrated sulfuric acid with the mass fraction of 98.3% according to the volume ratio of 1:9, and the mixed solution of formaldehyde and concentrated sulfuric acid is contained in the reaction holes 2 by 0.9mL. The polycyclic aromatic hydrocarbon sample bottle contains polycyclic aromatic hydrocarbon standard solution which is naphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]And (3) dissolving perylene in n-hexane to obtain a mixed standard solution. The number of the polycyclic aromatic hydrocarbon sample bottles is 6, namely a first polycyclic aromatic hydrocarbon sample bottle 10, a second polycyclic aromatic hydrocarbon sample bottle 11, a third polycyclic aromatic hydrocarbon sample bottle 12, a fourth polycyclic aromatic hydrocarbon sample bottle 13, a fifth polycyclic aromatic hydrocarbon sample bottle 14 and a sixth polycyclic aromatic hydrocarbon sample bottle 15. The concentration of the polycyclic aromatic hydrocarbon standard substance solution in the first polycyclic aromatic hydrocarbon sample bottle 10 is 0.25 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the second polycyclic aromatic hydrocarbon sample bottle 11 is 0.5 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the third polycyclic aromatic hydrocarbon sample bottle 12 is 1 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the fourth polycyclic aromatic hydrocarbon sample bottle 13 is 5 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the fifth polycyclic aromatic hydrocarbon sample bottle 14 is 10 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the sixth polycyclic aromatic hydrocarbon sample bottle 15 is 50 mug/mL. The volume of the polycyclic aromatic hydrocarbon sample bottles is 2mL, and each polycyclic aromatic hydrocarbon sample bottle contains 1mL of polycyclic aromatic hydrocarbon standard substance solution. The reaction disk 1 and the polycyclic aromatic hydrocarbon sample bottle are arranged inside the box body 8, and the cover body 9 is hinged with the box body 8.
Example 2
The embodiment provides a method for detecting polycyclic aromatic hydrocarbon pollutants in soil, which comprises the following steps,
s1, taking a soil sample, air-drying, grinding, sieving with a 20-target standard sieve to obtain a ground soil sample, taking 0.1g of the ground soil sample into a 10mL glass centrifuge tube, adding 3mL of dichloromethane into the ground soil sample, vibrating for 5min for extraction, centrifuging at 2000rpm for 5min, transferring the supernatant into a clean glass centrifuge tube with scales by using a suction tube, repeating the steps for three times, merging the supernatant, putting the centrifuge tube containing an extract into water at 40 ℃, heating and concentrating, and then fixing the volume to 0.1mL by using dichloromethane to obtain a sample solution to be detected.
S2, mixing a formaldehyde solution with the mass fraction of 37% with concentrated sulfuric acid with the mass fraction of 98.3% according to the volume ratio of 1:1000 to obtain a mixed solution of formaldehyde and concentrated sulfuric acid; s1 is obtainedAdding 0.1mL of the sample solution to be tested into 0.9mL of mixed solution of formaldehyde and concentrated sulfuric acid, observing whether dark green polymer is generated, if no dark green polymer is generated, indicating that the amount of polycyclic aromatic hydrocarbon in the soil sample is lower than 0.5mg/kg, and if the dark green polymer is generated, respectively taking 0.25 mug/mL, 0.5 mug/mL, 1 mug/mL, 5 mug/mL, 10 mug/mL and 50 mug/mL of polycyclic aromatic hydrocarbon standard substance solution, wherein 0.1mL of polycyclic aromatic hydrocarbon standard substance solution is added into 0.9mL of mixed solution of formaldehyde and concentrated sulfuric acid, and the polycyclic aromatic hydrocarbon standard substance solution is naphthalene, acenaphthylene, dihydroacenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene and benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]And (3) dissolving perylene in methylene dichloride to obtain a mixed standard solution, and comparing the amount of the dark green polymer generated by the sample solution to be detected with the amount of the dark green polymer generated by the 6 polycyclic aromatic hydrocarbon standard solution with different concentrations, so as to determine the approximate concentration of polycyclic aromatic hydrocarbon in soil.
S3, after detection is completed, adding 2mL of saturated sodium hydroxide solution to neutralize the concentrated sulfuric acid.
The embodiment also provides a kit for detecting polycyclic aromatic hydrocarbon, which comprises a box body 8 and a cover body 9 arranged on the box body 8, and further comprises a reaction plate 1 and a polycyclic aromatic hydrocarbon sample bottle, wherein 96 reaction holes 2 are formed in the reaction plate 1, mixed solution of formaldehyde and concentrated sulfuric acid is contained in the reaction holes 2, wherein the mixed solution of formaldehyde and concentrated sulfuric acid is obtained by mixing formaldehyde solution with the mass fraction of 37% and concentrated sulfuric acid with the mass fraction of 98.3% according to the volume ratio of 1:1000, and 0.9mL of mixed solution of formaldehyde and concentrated sulfuric acid is contained in the reaction holes 2. The polycyclic aromatic hydrocarbon sample bottle contains polycyclic aromatic hydrocarbon standard solution which is naphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene,Dibenzo [ a, h]Anthracene and benzo [ g, h, i]Perylene is dissolved in methylene chloride to obtain mixed standard solution. The number of the polycyclic aromatic hydrocarbon sample bottles is 6, namely a first polycyclic aromatic hydrocarbon sample bottle 10, a second polycyclic aromatic hydrocarbon sample bottle 11, a third polycyclic aromatic hydrocarbon sample bottle 12, a fourth polycyclic aromatic hydrocarbon sample bottle 13, a fifth polycyclic aromatic hydrocarbon sample bottle 14 and a sixth polycyclic aromatic hydrocarbon sample bottle 15. The concentration of the polycyclic aromatic hydrocarbon standard substance solution in the first polycyclic aromatic hydrocarbon sample bottle 10 is 0.25 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the second polycyclic aromatic hydrocarbon sample bottle 11 is 0.5 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the third polycyclic aromatic hydrocarbon sample bottle 12 is 1 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the fourth polycyclic aromatic hydrocarbon sample bottle 13 is 5 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the fifth polycyclic aromatic hydrocarbon sample bottle 14 is 10 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the sixth polycyclic aromatic hydrocarbon sample bottle 15 is 50 mug/mL. The volume of the polycyclic aromatic hydrocarbon sample bottles is 2mL, and each polycyclic aromatic hydrocarbon sample bottle contains 1mL of polycyclic aromatic hydrocarbon standard substance solution.
The kit for detecting the polycyclic aromatic hydrocarbon also comprises a strong alkali sample bottle 4, a liquid-transferring gun 5, a gun head 6 matched with the liquid-transferring gun 5 and two pairs of latex gloves 7; wherein, the strong alkali sample bottle 4 comprises 100g of sodium hydroxide solid with the volume of 60mL; the range of the pipette 5 is 200 mu L; 100 gun heads matched with the pipetting gun are provided; the cover body 9 can be opened and closed and is covered on the box body 8, the cover body 9 is hinged with the box body 8, the box body 8 comprises a liner 3 with a groove, and the liner is used for fixing the reaction disk 1, the polycyclic aromatic hydrocarbon sample bottle, the strong base sample bottle 4, the liquid-transfering gun 5, the gun head 6 matched with the liquid-transfering gun 5 and the latex glove 7.
Example 3
The embodiment provides a method for detecting polycyclic aromatic hydrocarbon pollutants in soil, which comprises the following steps,
s1, taking a soil sample, air-drying, grinding, sieving with a 20-target standard sieve to obtain a ground soil sample, taking 0.1g of the ground soil sample into a 10mL glass centrifuge tube, adding 3mL of dichloromethane into the ground soil sample, vibrating for 5min for extraction, centrifuging at 2000rpm for 5min, transferring the supernatant into a clean glass centrifuge tube with scales by using a suction tube, repeating the steps for three times, merging the supernatant, putting the centrifuge tube containing an extract into water at 40 ℃, heating and concentrating, and then fixing the volume to 0.1mL by using dichloromethane to obtain a sample solution to be detected.
S2, mixing a formaldehyde solution with the mass fraction of 37% with concentrated sulfuric acid with the mass fraction of 98.3% according to the volume ratio of 1:550 to obtain a mixed solution of formaldehyde and concentrated sulfuric acid; adding 0.1mL of the sample solution to be detected obtained in the step S1 into 0.9mL of a mixed solution of formaldehyde and concentrated sulfuric acid, observing whether dark green polymers are generated, if no dark green polymers are generated, indicating that the amount of polycyclic aromatic hydrocarbon in the soil sample is lower than 0.5mg/kg, and if the dark green polymers are generated, respectively taking 0.25 mug/mL, 0.5 mug/mL, 1 mug/mL, 5 mug/mL, 10 mug/mL and 50 mug/mL of polycyclic aromatic hydrocarbon standard substance solution, wherein 0.1mL of polycyclic aromatic hydrocarbon standard substance solution is added into 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid, and the polycyclic aromatic hydrocarbon standard substance solution is naphthalene, acenaphthylene, dihydro acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]And (3) dissolving perylene in methylene dichloride to obtain a mixed standard solution, and comparing the amount of the dark green polymer generated by the sample solution to be detected with the amount of the dark green polymer generated by the 6 polycyclic aromatic hydrocarbon standard solution with different concentrations, so as to determine the approximate concentration of polycyclic aromatic hydrocarbon in soil.
S3, after detection is completed, adding 2mL of saturated potassium hydroxide solution, and neutralizing concentrated sulfuric acid.
The embodiment also provides a kit for detecting polycyclic aromatic hydrocarbon, which comprises a box body 8 and a cover body 9 arranged on the box body 8, and further comprises a reaction plate 1 and a polycyclic aromatic hydrocarbon sample bottle, wherein 96 reaction holes 2 are formed in the reaction plate 1, mixed solution of formaldehyde and concentrated sulfuric acid is contained in the reaction holes 2, wherein the mixed solution of formaldehyde and concentrated sulfuric acid is obtained by mixing formaldehyde solution with the mass fraction of 37% and concentrated sulfuric acid with the mass fraction of 98.3% according to the volume ratio of 1:550, and 0.9mL of mixed solution of formaldehyde and concentrated sulfuric acid is contained in the reaction holes 2. Polycyclic aromatic hydrocarbon sample bottleWherein the polycyclic aromatic hydrocarbon standard substance solution is naphthalene, acenaphthylene dihydrogen, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]Perylene is dissolved in methylene chloride to obtain mixed standard solution. The number of the polycyclic aromatic hydrocarbon sample bottles is 6, namely a first polycyclic aromatic hydrocarbon sample bottle 10, a second polycyclic aromatic hydrocarbon sample bottle 11, a third polycyclic aromatic hydrocarbon sample bottle 12, a fourth polycyclic aromatic hydrocarbon sample bottle 13, a fifth polycyclic aromatic hydrocarbon sample bottle 14 and a sixth polycyclic aromatic hydrocarbon sample bottle 15. The concentration of the polycyclic aromatic hydrocarbon standard substance solution in the first polycyclic aromatic hydrocarbon sample bottle 10 is 0.25 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the second polycyclic aromatic hydrocarbon sample bottle 11 is 0.5 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the third polycyclic aromatic hydrocarbon sample bottle 12 is 1 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the fourth polycyclic aromatic hydrocarbon sample bottle 13 is 5 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the fifth polycyclic aromatic hydrocarbon sample bottle 14 is 10 mug/mL, the concentration of the polycyclic aromatic hydrocarbon standard substance solution in the sixth polycyclic aromatic hydrocarbon sample bottle 15 is 50 mug/mL. The volume of the polycyclic aromatic hydrocarbon sample bottles is 2mL, and each polycyclic aromatic hydrocarbon sample bottle contains 1mL of polycyclic aromatic hydrocarbon standard substance solution.
The kit for detecting the polycyclic aromatic hydrocarbon also comprises a strong alkali sample bottle 4, a liquid-transferring gun 5, a gun head 6 matched with the liquid-transferring gun 5 and two pairs of latex gloves 7; wherein, the strong alkali sample bottle 4 comprises 100g of potassium hydroxide solid with the volume of 60mL; the range of the pipette 5 is 200 mu L; 100 gun heads matched with the pipetting gun are provided; the cover body 9 can be opened and closed and is covered on the box body 8, the cover body 9 is hinged with the box body 8, the box body 8 comprises a liner 3 with a groove, and the liner is used for fixing the reaction disk 1, the polycyclic aromatic hydrocarbon sample bottle, the strong base sample bottle 4, the liquid-transfering gun 5, the gun head 6 matched with the liquid-transfering gun 5 and the latex glove 7.
Experimental example 1
The soil adopted in the experimental example is taken from a site polluted by some polycyclic aromatic hydrocarbon and petroleum hydrocarbon in the south, and the site is repaired by adopting a thermal desorption technology.
Taking a soil sample before restoration, and respectively adopting the detection methods in the examples 1-3 and the kit for detecting the polycyclic aromatic hydrocarbon to detect the concentration of the polycyclic aromatic hydrocarbon in the soil, wherein the result is that the dark green polymer is generated, and the quantity of the dark green polymer generated in the examples 1-3 is similar to that of the dark green polymer generated by the polycyclic aromatic hydrocarbon standard product with the concentration of 50 mug/mL in the 6 th sample bottle, so that the estimated value of the concentration of the polycyclic aromatic hydrocarbon in the soil is 50mg/kg. And detecting the concentration of the polycyclic aromatic hydrocarbon in the soil sample before restoration by adopting a GC-MS instrument, wherein the detection result is that the total concentration of the polycyclic aromatic hydrocarbon is 48.9mg/kg.
And (3) taking the soil with the same pollution point repaired by the thermal desorption technology, detecting the concentration of the polycyclic aromatic hydrocarbon in the soil by adopting the detection method in the embodiment 1-3 and the kit for detecting the polycyclic aromatic hydrocarbon, wherein no black green precipitate is generated as a result, detecting the concentration of the polycyclic aromatic hydrocarbon in the repaired soil sample by adopting a GC-MS instrument, and the detection result is that the total concentration of the polycyclic aromatic hydrocarbon is 0.41mg/kg. The result shows that the polycyclic aromatic hydrocarbon substances are basically treated completely after the thermal desorption treatment of the polluted land soil, and the repairing effect is good.
Experimental example 2
The soil adopted in the experimental example is taken from a polycyclic aromatic hydrocarbon polluted site in certain city in northwest, the site is repaired by adopting a chemical oxidation technology, the oxidant is persulfate, the ectopic oxidation is adopted, and the maintenance time is 21 days. And (3) adding an oxidant into the polluted soil, fully and uniformly mixing, adding water for maintenance, sampling on days 1, 7, 14 and 21 respectively, and measuring the concentration of the polycyclic aromatic hydrocarbon pollutant in the soil. The oxidation technique was evaluated using the detection methods and kits of examples 1-3, and the removal rates of polycyclic aromatic hydrocarbons were 15.34%, 62.26%, 70.87% and 78.69% on days 1, 7, 14 and 21, respectively, indicating that the detection methods and kits can rapidly evaluate the removal rates of PAHs by chemical oxidation techniques.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (7)
1. A method for detecting polycyclic aromatic hydrocarbon pollutants in soil is characterized by comprising the steps of,
s1, adding an extractant into a soil sample, concentrating and fixing the volume to obtain a sample solution to be detected;
s2, mixing the sample solution to be detected with a mixed solution of formaldehyde and concentrated sulfuric acid, observing whether a dark green polymer is generated, if no dark green polymer is generated, indicating that the amount of polycyclic aromatic hydrocarbon in the soil sample is lower than 0.5mg/kg, and if the dark green polymer is generated, comparing the amount of the generated dark green polymer with the amount of the dark green polymer generated by the reaction of the polycyclic aromatic hydrocarbon standard substance solution with different concentrations with the mixed solution of formaldehyde and concentrated sulfuric acid to obtain the concentration of the polycyclic aromatic hydrocarbon in the soil;
wherein the mixed solution of formaldehyde and concentrated sulfuric acid is obtained by mixing formaldehyde solution and concentrated sulfuric acid according to the volume ratio of 1:9-1:1000; the mass fraction of the formaldehyde solution is 37%, and the mass fraction of the concentrated sulfuric acid is 98.3%;
mixing each 0.1mL of the sample solution to be tested with 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid; mixing 0.1mL of the polycyclic aromatic hydrocarbon standard substance solution with 0.9mL of the mixed solution of formaldehyde and concentrated sulfuric acid;
the polycyclic aromatic hydrocarbon standard substance solution is naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]Mixed standard solutions of perylene.
2. The method for detecting polycyclic aromatic hydrocarbon contaminants in soil according to claim 1, wherein in step S1, the extractant is one or two of n-hexane and dichloromethane; the volume is determined by adding the extractant according to the ratio of the mass (g) of the soil sample to the volume (mL) =1:1 of the extract.
3. The method for detecting polycyclic aromatic hydrocarbon contaminants in soil according to claim 1, wherein the concentration of the polycyclic aromatic hydrocarbon standard solution is 0.25 μg/mL, 0.5 μg/mL, 1 μg/mL, 5 μg/mL, 10 μg/mL and 50 μg/mL, respectively.
4. The method for detecting polycyclic aromatic hydrocarbon contaminants in soil according to claim 1, further comprising the steps of drying, grinding and sieving the soil sample through a 20 mesh sieve before adding the extractant to the soil sample.
5. The method of claim 1 to 4, further comprising the step of adding a strong alkali solution after the detection, wherein the strong alkali is one or both of sodium hydroxide and potassium hydroxide.
6. Kit for polycyclic aromatic hydrocarbon detects, including box body (8) and lid (9) of setting on box body (8), its characterized in that still includes:
the reaction plate (1) is provided with reaction holes (2), and the reaction holes (2) are filled with mixed solution of formaldehyde and concentrated sulfuric acid;
the polycyclic aromatic hydrocarbon sample bottle is used for containing polycyclic aromatic hydrocarbon standard substance solutions with different concentrations;
wherein the polycyclic aromatic hydrocarbon standard substance solution is naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a ]]Anthracene (anthracene),Benzo [ k ]]Fluoranthene, benzo [ b ]]Fluoranthene, benzo [ a ]]Pyrene, indeno [123-c, d]Pyrene, dibenzo [ a, h]Anthracene and benzo [ g, h, i]Perylene derivativesThe standard solution was mixed.
7. The kit for polycyclic aromatic hydrocarbon detection according to claim 6, further comprising a strong base sample bottle (4), a pipette gun (5), a gun head (6) matched with the pipette gun (5), and a glove (7); wherein, the strong alkali sample bottle (4) contains strong alkali solid.
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