Method for determining petroleum solvent in solid waste

CN119985381APending Publication Date: 2025-05-13江苏康达检测技术股份有限公司
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Patent Information

Application Number
CN202411681919.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-22
Publication Date
2025-05-13

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Abstract

The invention discloses a method for determining a petroleum solvent in solid waste, and the method comprises the following steps: collecting a sample, and carrying out homogenization treatment on the collected sample; carrying out dehydration treatment on the homogenized sample by adopting a first dehydrating agent; performing oscillation extraction on the dehydrated sample by adopting a first extraction solvent; carrying out purification and leaching treatment on a product subjected to oscillation extraction to obtain a primary liquid to be detected; determining a final to-be-detected solution according to the color condition of the preliminary to-be-detected solution; and injecting the final to-be-detected liquid into an infrared oil detector, and detecting the content of the petroleum solvent in the solid waste based on an infrared spectroscopic analysis method. According to the method, the petroleum solvent in the solid waste can be effectively detected, and the detection efficiency and accuracy are improved by optimizing oscillation extraction, chromatographic purification and infrared spectrum conditions.
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Description

Technical Field

[0001] The invention relates to the technical field of chemical detection, in particular to a method for determining petroleum solvents in solid wastes. Background Art

[0002] Petroleum solvents, i.e. recyclable petroleum hydrocarbons, contain alkanes, cycloalkanes and a small amount of aromatics, and are widely used in the petroleum and related industries. They seriously pollute water, soil and air, affect the growth of plants and animals, and contain toxic substances such as polycyclic aromatic hydrocarbons, benzene series, phenols, etc., which pose a threat to human health, including carcinogenic risks. Petroleum solvents have been listed as hazardous wastes, and accurate determination of petroleum solvents in solid wastes is crucial for the identification of hazardous wastes.

[0003] At present, there are few studies on the detection methods of petroleum solvents in solid waste in China, which mainly refer to the determination methods of the total amount of petroleum hydrocarbons in water quality and soil, including weight method, ultraviolet spectrophotometry, infrared spectroscopy and gas chromatography. Among them, infrared spectroscopy is the most commonly used due to its high sensitivity and unaffected by the type of petroleum hydrocarbons.

[0004] In addition, the extraction methods for the determination of the total amount of petroleum hydrocarbons mainly include ultrasonic extraction, Soxhlet extraction, oscillation and accelerated solvent extraction. These methods each have their own advantages and disadvantages. The ultrasonic extraction method has good effect but poor stability; the Soxhlet extraction method has stable effect but takes a long time and uses a large amount of solvent; the oscillation method has stable effect, short time and uses a small amount of solvent; the accelerated solvent extraction method also has stable effect, short time and uses a small amount of solvent, but the equipment is expensive and the operation is complicated.

[0005] Furthermore, the detection methods of petroleum solvents in solid waste in the current effective standards include: Appendix O of the "Identification Standard for Hazardous Wastes - Identification of Toxic Substance Content" (GB5085.6-2007) and the "Standard Test Method for Urban Sludge" (CJ / T 221-2023); both of the above schemes have limitations in practical applications. The technical parameters of the former are not quantified, and the banned carbon tetrachloride is used as the extraction solvent; the latter is mainly suitable for urban sludge, not for solid waste with complex matrices, and the pretreatment is time-consuming and the solvent consumption is large, which is harmful to the environment and experimenters. Summary of the invention

[0006] The object of the present invention is to provide a method for determining petroleum solvents in solid wastes, thereby solving all or one of the above problems existing in the prior art.

[0007] In order to solve the above technical problems, the specific technical solutions of the present invention are as follows: The present invention provides a method for determining petroleum solvent in solid waste, comprising the following steps: Sample preparation steps: Collecting samples, homogenizing the collected samples; dehydrating the homogenized samples with a first dehydrating agent; oscillating and extracting the dehydrated samples with a first extraction solvent; purifying and eluting the products after the oscillation extraction to obtain a preliminary test solution; and determining a final test solution according to the color of the preliminary test solution; Determination steps: The final test liquid is injected into an infrared oil measuring instrument, and the content of petroleum solvent in the solid waste is measured based on infrared spectroscopy.

[0008] In one embodiment, the homogenization process comprises: The sample is placed on a clean and dry tray, and then impurities in the sample are removed; the volume of the sample is reduced according to the shape of the sample.

[0009] In one embodiment, the dehydration process comprises: Weighing a first mass of the homogenized sample into a blue-capped glass bottle; Then, the first dehydrating agent is added into the blue-capped glass bottle, and the mixture is stirred and mixed thoroughly.

[0010] In one embodiment, the oscillation extraction comprises: After the thorough stirring and mixing, a second mass of the first extraction solvent is added to the blue-capped glass bottle; then, the blue-capped glass bottle is flipped and shaken at a first rotation speed for a first time period and then allowed to stand.

[0011] In one embodiment, the purification and elution treatment comprises: Taking a third mass of supernatant from the liquid after standing; The supernatant is purified by a silica gel purification column, and the third mass of the first extraction solvent is added for elution; after elution, all filtrates are collected as the preliminary test solution.

[0012] In one embodiment, determining the final test liquid according to the color of the preliminary test liquid includes: When the color of the preliminary test liquid is darker, a magnesium silicate adsorption column is used to perform a re-purification operation on the preliminary test liquid.

[0013] In one embodiment, the complex purification operation includes: The preliminary test solution is measured and passed through the magnesium silicate adsorption column. When passing through the magnesium silicate adsorption column, the fourth mass of filtrate initially flowing out is discarded, and the remaining filtrate is collected as the final test solution.

[0014] In one embodiment, the determining step further comprises: Prepare a series of standard curve solutions with different mass concentrations; The standard curve solutions with different mass concentrations were sequentially injected into the infrared oil analyzer, and a 4 cm long quartz cuvette was used at a wave number of 2950 cm -1 Determine the absorbance of each of the standard curve series solutions; A standard curve is drawn with the mass concentration of the target substance as the abscissa and the absorbance as the ordinate.

[0015] In one embodiment, it also includes: When processing the first number of samples or each batch of samples, perform a blank run, a replicate analysis, and a blank spiked sample analysis.

[0016] In one embodiment, the first mass is 10 g; The first dehydrating agent is anhydrous sodium sulfate; The second mass is 100 mL; The first extraction solvent is tetrachloroethylene; The first speed is (30±2) r / min; The first duration is 3 hours; The third mass is 10 mL; The fourth mass is 5 mL.

[0017] The beneficial effects of the technical solution of the present invention are: The method for determining petroleum solvents in solid wastes described in the present invention can effectively detect petroleum solvents (recoverable petroleum hydrocarbons) in solid wastes, and improves detection efficiency and accuracy by optimizing oscillation extraction, chromatography purification and infrared spectroscopy conditions. It can be used as a supplement to existing standards for hazardous waste identification in laboratories. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0019] Figure 1 1 is a schematic flow chart of a method for determining petroleum solvents in solid wastes according to Example 1 of the present invention; Figure 2It is a logical flow chart of the method for determining petroleum solvents in solid wastes described in Example 1 of the present invention. DETAILED DESCRIPTION

[0020] The preferred embodiments of the present invention are described in detail below in conjunction with the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making a clearer and more definite definition of the protection scope of the present invention.

[0021] In the description of the present invention, it should be noted that the embodiments described in the present invention are only part of the embodiments of the present invention, rather than all of the embodiments; based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in the field without making creative work are within the scope of protection of the present invention.

[0022] The terms "first", "second", etc. in the specification and claims of this article and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchanged where appropriate, so that the embodiments of this article described here can be implemented in an order other than those illustrated or described here. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions, for example, a process, method, device, product or equipment that includes a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or equipment.

[0023] In the description of the present invention, it should be noted that: IR, (Infrared Absorption Spectrometry), is infrared spectroscopy; ODS, (Ozone Depleting Substances), is a substance that depletes the ozone layer.

[0024] 1. In the embodiments of the present invention, the following listed instruments, reagents and conditions are all used as an implementation method, and the implementation method can be adapted and adjusted according to the implementation environment, objectives or conditions of the method in this embodiment.

[0025] 2. In the embodiments of the present invention, the instruments and equipment used are as follows: 1. Infrared oil tester: can measure oil at 2950cm -1 The absorbance is measured at 400 nm and is equipped with a 4 cm quartz cuvette.

[0026] 2. Flip oscillator: the rotation speed is (30±2) r / min.

[0027] 3. Analytical balance: sensitivity 0.01g.

[0028] 4. Other common laboratory instruments and equipment.

[0029] 3. In the embodiments of the present invention, the reagent materials and their standards used are as follows: 1. Tetrachloroethylene (C2Cl4), n-hexadecane (C 16 H 34 ), isooctane (C8H 18 ), chlorobenzene (C6H5Cl), all of which were chromatographically pure. The preparation process and storage conditions were as follows: 15.0 mL of n-hexadecane, 15.0 mL of isooctane and 10.0 mL of chlorobenzene were added into a 50 mL bottle with a glass stopper, the stopper was tightly closed to avoid loss of sample due to volatilization, and the sample was stored below 4°C.

[0030] 2. Reference oil.

[0031] 3. The preparation process and storage conditions of the standard stock solution are as follows: take 0.5 mL of the reference oil and add it to a 100 mL weighed volumetric flask, immediately cover the flask tightly; weigh it and dilute it to the scale with tetrachloroethylene.

[0032] 4. The preparation process of 200 mg / L standard working solution is as follows: accurately transfer an appropriate amount of standard stock solution into a 100 mL volumetric flask, dilute to the scale with tetrachloroethylene, and prepare a standard working solution with a mass concentration of 200 mg / L.

[0033] 5. Silica gel: 200~100 mesh.

[0034] 6. Silica gel purification column: the preparation process is as follows: fill a small amount of glass wool at the outlet of a glass column with an inner diameter of 10mm and a length of about 200mm, dissolve silica gel and tetrachloroethylene in a 1:1 ratio and slowly pour into the glass column, tapping gently while pouring, and the filling height is about 80mm; activate the silica gel purification column with 10mL of tetrachloroethylene before use.

[0035] 7. Calibration of silica gel purification column: Take 1 mL corn oil and place it in a 100 mL weighed volumetric flask to prepare corn oil stock solution, weigh it, dilute it to the scale with tetrachloroethylene, and shake it well; prepare the target concentration dilution solution as needed; take 10 mL of the diluted corn oil solution and pass it through the silica gel purification column, then add 10 mL of tetrachloroethylene for elution, collect all the filtrate and use a 4 cm quartz cuvette at 2950 cm -1 Measure the absorbance at the sample and compare it with the content before purification to determine the adsorption capacity of the silica gel.

[0036] 8. Anhydrous sodium sulfate (Na2SO4), storage conditions: heat at 450℃ in a muffle furnace for 4 hours, put into a ground glass bottle after cooling slightly, and store in a desiccator.

[0037] 9. Quartz sand 100~20 mesh, storage conditions: heat in a muffle furnace at 450℃ for 4 hours, put into a ground glass bottle after cooling slightly, and store in a desiccator.

[0038] 10. Magnesium silicate (MgSiO3): 100~60 mesh.

[0039] 11. The preparation method of magnesium silicate adsorption column is as follows: fill a small amount of glass wool at the outlet of a glass column with an inner diameter of 10 mm and a length of about 200 mm, slowly pour magnesium silicate into the glass column, tapping gently while pouring, and the filling height is about 80 mm.

[0040] This embodiment provides a method for determining petroleum solvents in solid wastes. Figure 1 and Figure 2 As shown, the following steps are included: S100, sample pretreatment steps: In this step, a sample is prepared, the prepared sample is weighed and dehydrated by adding an appropriate amount of anhydrous magnesium sulfate, tetrachloroethylene is used as an extraction solvent for oscillation extraction, and the supernatant is removed for purification and elution treatment to obtain the corresponding test solution, which is as follows: S101. Sample collection: Collect and preserve solid waste samples in accordance with the relevant provisions of the Technical Specifications for Sampling and Preparation of Industrial Solid Waste (HJ / T 20-1998) and the Technical Specifications for Identification of Hazardous Waste (HJ 298-2019); Specifically, samples were stored in clean brown glass bottles with stoppers and ground-mouths, and the bottles were kept sealed, light-proof, and refrigerated below 4°C. If samples cannot be analyzed in time, they were placed in a refrigerated environment below 4°C and stored in a sealed and light-proof environment for no more than 10 days.

[0041] S102, sample homogenization: the collected solid waste samples are placed on a clean and dried tray, and then impurities are removed; then, according to the specific form of the solid waste samples, corresponding measures are taken to reduce their volume; Specifically, measures to reduce the volume include, but are not limited to, grinding, shearing, tearing or other effective means to ensure that the sample can reach a sufficiently uniform state.

[0042] S103. Sample preparation: Accurately weigh about 10g (accurate to 0.01g) of the above-mentioned uniformly treated sample and place it in a 250mL blue-capped glass bottle; then, add an appropriate amount of anhydrous sodium sulfate to the bottle and stir it thoroughly to ensure uniform mixing; after stirring, add 100mL of tetrachloroethylene as the extraction solvent; then flip and oscillate the glass bottle at a speed of (30±2) revolutions per minute for 3 hours, and then let it stand; from the liquid after standing, take out 10mL of the supernatant, purify it through a silica gel purification column, and add 10mL of tetrachloroethylene for elution; after elution, collect all the filtrate as the test liquid.

[0043] S104, purity judgment: observe the color of the liquid to be tested. If the color is dark, a magnesium silicate adsorption column is used to further purify the sample that has been purified by a silica gel column. Specifically, a proper amount of solution was measured and passed through the magnesium silicate adsorption column. During this process, the first 5 mL of filtrate was discarded, and the remaining filtrate was collected as the final test solution.

[0044] S105. Preparation of blank sample: Use quartz sand instead of sample and prepare laboratory blank sample according to the same steps as the preparation of the test solution.

[0045] S200, determination steps: In this step, the eluate is injected into the infrared oil analyzer using a quartz cuvette of 4 cm in length at a wave number of 2950 cm -1 The absorbance is measured at the position of the infrared spectrometer; the petroleum solvent content in the solid waste is measured according to the relevant requirements of the infrared spectroscopy analysis method, as follows: S201, preparing a series of standard curve solutions: measuring a certain amount of standard working solutions into a plurality of 25 mL volumetric flasks, and then using tetrachloroethylene to dilute the solutions in the volumetric flasks to the scale lines, thereby preparing a series of standard curve solutions containing at least 8 different concentration points, and the reference concentration range of the series of standard curve solutions is set from 0.00 mg / L to 200 mg / L; Specifically, the reference concentration ranges of the standard curve series solutions are 0.00 mg / L, 4.00 mg / L, 8.00 mg / L, 40.0 mg / L, 80.0 mg / L, 120 mg / L, 160 mg / L and 200 mg / L, respectively.

[0046] S202, draw a standard curve: sequentially inject a series of standard curve solutions with different mass concentrations into the infrared oil tester, use a quartz cuvette with a length of 4 cm, and draw a standard curve at a wave number of 2950 cm -1The absorbance of each solution is measured at a certain point; subsequently, a standard curve is drawn with the mass concentration of the target substance as the abscissa and the measured absorbance as the ordinate; Specifically, during the measurement, if the absorbance of a solution is found to exceed the linear measurement range of the infrared oil analyzer, the sample needs to be appropriately diluted and the absorbance needs to be re-measured and analyzed.

[0047] S203, sample determination: Based on the above steps, the sample is determined according to the same instrument analysis conditions and steps as those for drawing the standard curve.

[0048] S203, blank sample determination: Based on the above steps, a blank sample determination is performed according to the same instrument analysis conditions and steps as the sample determination.

[0049] S204. Calculation of the content (%) of petroleum solvents (recoverable petroleum hydrocarbons) in solid wastes: Specifically, the calculation formula is: ; in: It is the content of petroleum solvent (i.e. recoverable petroleum hydrocarbon) in solid waste, in %; The mass concentration of petroleum solvent in the sample calculated based on the standard curve, in mg / L; V is the volume of the extraction solvent added during sample preparation, mL; is the dilution multiple of the extract; is the mass of the solid waste sample, in g; 0.0002 is the conversion factor; It should be noted that the number of decimal places in the calculated result is consistent with the detection limit of the method, and a maximum of three significant digits are retained.

[0050] S300, backup steps: In this step, all used utensils are placed in a fume hood to allow them to evaporate and dry naturally, and then thoroughly cleaned. At the same time, the waste and waste liquid generated during the previous measurement process are collected and properly stored, and finally sent to a professional treatment unit with relevant qualifications for safe disposal.

[0051] It should be noted that in order to ensure the detection effect of this method, the following specifications are set: (1) When this method is used, if the sample size is 10 g, the extract volume is set to 100 mL, and a 4 cm quartz cuvette is used, the detection limit of the method is 0.0010%. The lower limit of determination, calculated as four times the detection limit, is 0.0040%.

[0052] (2) A laboratory blank test should be performed for every 20 samples or each batch (if there are less than 20 samples, it is considered as one batch). In the blank test, the concentration of the target substance should be lower than the detection limit of the method.

[0053] (3) A parallel sample analysis should be performed for every 20 samples or each batch (if there are less than 20 samples, it is considered as one batch), and the relative deviation of the measurement results between parallel samples should be controlled within 20%.

[0054] (4) A blank spiked sample analysis should be performed for every 20 samples or each batch (if there are less than 20 samples, it is considered as one batch), and the spiked sample recovery rate should be kept between 70% and 130%.

[0055] (5) The samples of the same batch should be measured using tetrachloroethylene from the same bottle. If the number of samples is large, multiple bottles of tetrachloroethylene should be mixed evenly before use.

[0056] (6) The correlation coefficient of the calibration curve should be 0.999 or above. Each batch of samples needs to be tested for the correction factor as follows: take an appropriate amount of standard working solution according to the required concentration, prepare a standard solution of appropriate concentration using tetrachloroethylene as the solvent, and perform the test according to the same measurement steps as the test sample; then, calculate the concentration of the standard solution according to the above calculation formula; if the relative error between the measured value and the standard value is within ±10%, the correction factor is considered to be applicable; if it exceeds this range, the correction factor needs to be re-measured and tested until the above conditions are met.

[0057] In summary, this method uses tetrachloroethylene to extract recoverable petroleum hydrocarbons from solid waste. After the extract is purified by silica gel, it is measured by infrared oil meter at 2950cm -1 The absorbance is measured at the site, thereby completing the determination of recoverable petroleum hydrocarbons in solid wastes such as sludge, waste residue, and garbage. This method improves the analysis efficiency and accuracy, simplifies the operation and saves solvents by optimizing pretreatment, analysis conditions and refining fuzzy definitions.

[0058] It should be noted that the above examples are only for explaining the present invention and cannot limit the protection scope of the present invention.

[0059] Different from the prior art, the method for determining petroleum solvents in solid wastes of the present application can effectively detect petroleum solvents (recoverable petroleum hydrocarbons) in solid wastes. By optimizing the conditions of oscillation extraction, chromatography purification and infrared spectroscopy, the detection efficiency and accuracy are improved. The method can be used as a supplement to the existing standard (Appendix O of GB 5085.6-2007) for the identification of hazardous wastes in the laboratory.

[0060] It should be understood that in the various embodiments of this document, the size of the serial numbers of the above-mentioned processes does not mean the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this document.

[0061] It should also be understood that in the embodiments of this article, the term "and / or" is only a description of the association relationship of the associated objects, indicating that three relationships may exist. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in this article generally indicates that the associated objects before and after are in an "or" relationship.

[0062] Those of ordinary skill in the art will appreciate that the units and algorithm steps of each example described in conjunction with the embodiments disclosed herein can be implemented in electronic hardware, computer software, or a combination of the two. In order to clearly illustrate the interchangeability of hardware and software, the composition and steps of each example have been generally described in terms of function in the above description. Whether these functions are performed in hardware or software depends on the specific application and design constraints of the technical solution. Professional and technical personnel can use different methods to implement the described functions for each specific application, but such implementation should not be considered to be beyond the scope of this article.

[0063] Those skilled in the art can clearly understand that, for the convenience and brevity of description, the specific working processes of the systems, devices and units described above can refer to the corresponding processes in the aforementioned method embodiments and will not be repeated here.

[0064] In the several embodiments provided herein, it should be understood that the disclosed systems, devices and methods can be implemented in other ways. For example, the device embodiments described above are only schematic, for example, the division of the units is only a logical function division, and there may be other division methods in actual implementation, such as multiple units or components can be combined or integrated into another system, or some features can be ignored or not executed. In addition, the mutual coupling or direct coupling or communication connection shown or discussed can be an indirect coupling or communication connection through some interfaces, devices or units, or can be electrical, mechanical or other forms of connection.

[0065] The units described as separate components may or may not be physically separated, and the components shown as units may or may not be physical units, that is, they may be located in one place or distributed on multiple network units. Some or all of the units may be selected according to actual needs to achieve the purpose of the embodiments of this article.

[0066] In addition, each functional unit in each embodiment of this invention may be integrated into one processing unit, or each unit may exist physically separately, or two or more units may be integrated into one unit. The above integrated unit may be implemented in the form of hardware or in the form of software functional unit.

[0067] If the integrated unit is implemented in the form of a software functional unit and sold or used as an independent product, it can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of this article is essentially or the part that contributes to the prior art, or all or part of the technical solution can be embodied in the form of a software product, and the computer software product is stored in a storage medium, including a number of instructions to enable a computer device (which can be a personal computer, a server, or a network device, etc.) to perform all or part of the steps of the method described in each embodiment of this article. The aforementioned storage medium includes: U disk, mobile hard disk, read-only memory (ROM, Read-Only Memory), random access memory (RAM, Random Access Memory), disk or optical disk and other media that can store program codes.

[0068] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A method for determining petroleum solvents in solid waste, characterized in that: The following steps are involved: Sample preparation steps: Collecting samples and performing homogenization on the collected samples; and dehydrating the homogenized samples using a first dehydrating agent; The dehydrated sample is subjected to oscillation extraction using a first extraction solvent; the product after the oscillation extraction is purified and washed to obtain a preliminary test solution; and a final test solution is determined according to the color of the preliminary test solution; Determination steps: The final test liquid is injected into an infrared oil measuring instrument, and the content of petroleum solvent in the solid waste is measured based on infrared spectroscopy.

2. The method for determining petroleum solvent in solid waste according to claim 1, characterized in that: The homogenization process comprises: The sample is placed on a clean and dry tray, and then impurities in the sample are removed; the volume of the sample is reduced according to the shape of the sample.

3. The method for determining petroleum solvent in solid waste according to claim 1, characterized in that: The dehydration process comprises: Weighing a first mass of the homogenized sample into a blue-capped glass bottle; Then, the first dehydrating agent is added into the blue-capped glass bottle, and the mixture is stirred and mixed thoroughly.

4. The method for determining petroleum solvent in solid waste according to claim 3, characterized in that: The oscillation extraction comprises: After the thorough stirring and mixing, a second mass of the first extraction solvent is added to the blue-capped glass bottle; then, the blue-capped glass bottle is flipped and shaken at a first speed for a first time period and then allowed to stand.

5. The method for determining petroleum solvent in solid waste according to claim 4, characterized in that: The purification and elution treatment comprises: Taking a third mass of supernatant from the liquid after standing; The supernatant is purified by a silica gel purification column, and the third mass of the first extraction solvent is added for elution; after elution, all filtrates are collected as the preliminary test solution.

6. The method for determining petroleum solvent in solid waste according to claim 5, characterized in that: The step of determining the final liquid to be tested according to the color of the preliminary liquid to be tested comprises: When the color of the preliminary test liquid is darker, a magnesium silicate adsorption column is used to perform a re-purification operation on the preliminary test liquid.

7. The method for determining petroleum solvent in solid waste according to claim 6, characterized in that: The complex purification operation comprises: The preliminary test solution is measured and passed through the magnesium silicate adsorption column. When passing through the magnesium silicate adsorption column, the fourth mass of filtrate initially flowing out is discarded, and the remaining filtrate is collected as the final test solution.

8. The method for determining petroleum solvents in solid waste according to claim 1, characterized in that: The measuring step further comprises: Prepare a series of standard curve solutions with different mass concentrations; Sequentially inject the standard curve solutions with different mass concentrations into the infrared oil analyzer, use a 4 cm long quartz cuvette, and measure the oil at a wave number of 2950 cm -1 Determine the absorbance of each of the standard curve series solutions; A standard curve is drawn with the mass concentration of the target substance as the abscissa and the absorbance as the ordinate.

9. The method for determining petroleum solvent in solid waste according to claim 1, characterized in that: Also includes: When processing the first number of samples or each batch of samples, perform a blank run, a replicate analysis, and a blank spiked sample analysis.

10. The method for determining petroleum solvents in solid waste according to claim 7, characterized in that: The first mass is 10 g; The first dehydrating agent is anhydrous sodium sulfate; The second mass is 100 mL; The first extraction solvent is tetrachloroethylene; The first speed is 28-32 r / min; The first duration is 3 hours; The third mass is 10 mL; The fourth mass is 5 mL.