CN112684070B - Method for measuring semi-volatile organic compounds in solid waste - Google Patents
Method for measuring semi-volatile organic compounds in solid waste Download PDFInfo
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- CN112684070B CN112684070B CN202011550206.3A CN202011550206A CN112684070B CN 112684070 B CN112684070 B CN 112684070B CN 202011550206 A CN202011550206 A CN 202011550206A CN 112684070 B CN112684070 B CN 112684070B
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- 239000002910 solid waste Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 30
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- 238000001514 detection method Methods 0.000 claims abstract description 19
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- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 8
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 7
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- OCJBOOLMMGQPQU-RHQRLBAQSA-N 1,4-dichloro-2,3,5,6-tetradeuteriobenzene Chemical group [2H]C1=C([2H])C(Cl)=C([2H])C([2H])=C1Cl OCJBOOLMMGQPQU-RHQRLBAQSA-N 0.000 claims description 6
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- DPMZXMBOYHBELT-UHFFFAOYSA-N 1,3,5-trimethyl-1,3,5-triazinane Chemical compound CN1CN(C)CN(C)C1 DPMZXMBOYHBELT-UHFFFAOYSA-N 0.000 claims description 4
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- WNNPYVQKNPPTLA-UHFFFAOYSA-N n-[(dimethylamino)methyl]-n-methylformamide Chemical compound CN(C)CN(C)C=O WNNPYVQKNPPTLA-UHFFFAOYSA-N 0.000 claims description 4
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- PGTMTTGPWLZNQO-UHFFFAOYSA-N 2-dodecyl-1,3,5,7,9,11-hexaoxa-2,4,6,8,10,12-hexasilacyclododecane Chemical compound C(CCCCCCCCCCC)[SiH]1O[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH2]O1 PGTMTTGPWLZNQO-UHFFFAOYSA-N 0.000 claims description 3
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- GPAPPPVRLPGFEQ-UHFFFAOYSA-N 4,4'-dichlorodiphenyl sulfone Chemical compound C1=CC(Cl)=CC=C1S(=O)(=O)C1=CC=C(Cl)C=C1 GPAPPPVRLPGFEQ-UHFFFAOYSA-N 0.000 claims description 2
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- POLIXZIAIMAECK-UHFFFAOYSA-N 4-[2-(2,6-dioxomorpholin-4-yl)ethyl]morpholine-2,6-dione Chemical compound C1C(=O)OC(=O)CN1CCN1CC(=O)OC(=O)C1 POLIXZIAIMAECK-UHFFFAOYSA-N 0.000 description 2
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of detection, in particular to a method for measuring semi-volatile organic compounds in solid waste and application thereof. The method comprises the following steps: s1, collecting a solid waste sample; s2, preparing a standard sample; s3, pretreating a sample; the weight ratio of the sample to the diatomite is 1: (5-15) mixing, grinding to 120-160 meshes, then adding into an extraction tank, setting the extraction temperature to be 95-120 ℃, setting the extraction pressure to be 1300-1600Pa, setting the extraction time to be 5min, and setting the extraction solvent to be a mixed solution of dichloromethane and acetone, wherein the volume ratio of the dichloromethane to the acetone is 1:1, repeatedly extracting for 3 times to obtain an extracting solution; concentrating the extract to 2mL under reduced pressure by a rotary evaporator, activating by a solid phase extraction device, loading, leaching, eluting, concentrating to 1mL, adding 1 mu L of internal standard, rapidly sealing, and measuring; s4, placing the pretreated sample and the standard sample into a gas chromatography-mass spectrometer for detection; the gas chromatography mass spectrometer comprises at least a gas chromatography module and a mass spectrometry module.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for measuring semi-volatile organic compounds in solid waste.
Background
The Semi-volatile organic compound (Semi-Volatile Organic Compounds) is usually an organic compound having a boiling point of 24 to 400℃and a vapor pressure of (0.1 to 10 -7). Times.133.322 Pa. Along with the acceleration of urban process and the increasing of living standard of residents in China, the demand for corresponding resources is increased year by year, so that the total amount and types of solid wastes are in an ascending trend. Because the solid waste has the characteristics of large yield, dispersed sources, complex components, changeable morphology and properties and the like, the solid waste occupies a large amount of land and space resources in the stacking process, and harmful substances enter water, soil and atmosphere through rain wash and surface runoff, so that the original ecological structure is seriously damaged. Meanwhile, the solid waste releases volatile and semi-volatile organic pollutants due to insolation, and has the hidden trouble of secondary pollution caused by chemical reaction which occurs due to improper treatment mode, serious damage to ecological environment and influence on daily life of residents. From the current economic development condition and pollution trend of China, the monitoring of organic pollutants in solid waste is an important target for environmental monitoring.
The SVOCs in solid waste mainly comprise: total organic carbon, organophosphorus pesticides, organochlorine pesticides, chlorinated herbicides, polycyclic aromatic hydrocarbons, phthalates, polychlorinated biphenyls, phenols, and total petroleum hydrocarbons (> C13). SVOCs are important raw materials for organic chemical industries such as dyes, pharmaceuticals, pesticides, etc., and are widely used, and most of them have characteristics of 'three-way', low water solubility, lipophilicity, biological degradation resistance, etc., and are considered as persistent toxic compounds due to their high stability in the environment and accumulation in organisms.
The content of SVOCs in the solid waste is low, the sample is difficult to directly analyze and measure when not being treated, and trace components in the sample are usually required to be concentrated by an extraction means so as to reduce matrix interference and improve the accuracy and the sensitivity of the method. Soxhlet extraction is the most classical method for extracting nonpolar and semi-volatile trace organic pollutants, but has long extraction time and complex operation, and has been gradually replaced by more advanced extraction methods. Ultrasonic extraction is one of the simplest methods for analyzing and extracting organic pollutants in a solid matrix, and the method is simple and convenient to operate, but the extracted centrifugally separated organic matters are easy to introduce human errors and are not suitable for batch sample treatment. Along with the progress of the economic development level and the aggravation of pollution trend in China, the preparation of a method for efficiently and rapidly detecting the content of SVOCs in solid waste becomes a problem to be solved in the field.
Disclosure of Invention
The invention solves the problems of low extraction efficiency and poor reproducibility of the measurement result of the semi-volatile organic compounds in the solid waste sample in the prior art by providing the measurement method of the semi-volatile organic compounds in the solid waste, and realizes the efficient and accurate detection of the semi-volatile organic compounds in the solid waste.
The first aspect of the invention provides a method for determining semi-volatile organic compounds in solid waste, comprising the following steps:
S1, collecting a solid waste sample;
S2, preparing a standard sample;
S3, pretreating a sample;
S4, placing the pretreated sample and the standard sample into a gas chromatography-mass spectrometer for detection; the gas chromatography mass spectrometer comprises at least a gas chromatography module and a mass spectrometry module.
In a preferred embodiment, the diatomaceous earth in the step S3 is diatomaceous earth calcined at a high temperature.
In a preferred embodiment, the operating conditions of the gas chromatography module in step S4 are: selecting a polysiloxane gas chromatographic column; the temperature of the sample inlet is 290-310 ℃; the sample injection mode is split-flow sample injection; the carrier gas is high-purity helium; the gas chromatographic module adopts temperature programming to separate the target object to be detected.
In a preferred embodiment, the split ratio of the split sample is (3-10): 1.
In a preferred embodiment, the temperature programming conditions are: keeping at 45 ℃ for 2min; heating to 260 ℃ at a speed of 20 ℃/min for 0min, heating to 280 ℃ at a speed of 6 ℃/min for 0min, and heating to 310 ℃ at 10 ℃/min for 5min.
In a preferred embodiment, the polysiloxane gas chromatography column is an Agilent DB-5 30m 0.25mm 0.25 μm.
In a preferred embodiment, the conditions of the mass spectrometry module are: ion source EI, scanning ion range: 35-550amu, ion source temperature 220-240 ℃.
In a preferred embodiment, the internal standard comprises 1, 4-dichlorobenzene-d 4, naphthalene-d 8, acenaphthene-d 10, phenanthrene-d 10,-At least one of d12 and perylene-d 12.
In a preferred embodiment, the semi-volatile organic compound comprises bis (2-ethylhexyl) phthalate, phthalimide, 2, 6-bis (trimethylsiloxy) benzoic acid trimethylsilyl ester, dodecylcyclohexasiloxane, morpholine-3, 5-dione, aminoacetonitrile, chloromethyl thiocyanate, hexahydro-1, 3, 5-trimethyl-S-triazine, N- ((dimethylamino) methyl) -N-methylformamide, N, N-dimethylurea, trimethylurea, 2-amino-3-hydroxypyridine, 2-chloro-1, 3-thiazole-5-carbaldehyde, tributylamine, N-benzyldiethylamine, 2- (5-amino-3-oxo-3, 6-dihydro-2H-piperazin-1-yl) -acetamide, hexamethylenetetramine, ethylene glycol bis (2-aminoethylether) tetraacetic acid, acetone dimethylhydrazine, creatinine, N-propyl-2-methylpentyl-4-allyl-1-amine, 1-methyl-1, 3-thiazole-5-carbaldehyde, tributylamine, N-dimethyl-4-aminopyrimidine, N, N '-dimethylpropanamide, N, N-3-dimethylpropylamine, N, 3-dimethylpropylamine, N' -dimethylpropylamine, N, 3-dimethylpropylamine At least one of ethylenediamine tetraacetic acid dianhydride, N-dimethyl propenyl urea, 4' -dichloro diphenyl sulfone, 2-acetone bis (1-methyl ethyl) hydrazone, lysergic acid, N-ethyl-2, 3-diketopiperazine and propylimine.
In a second aspect, the invention provides the use of a method for determining semi-volatile organic compounds in solid waste, the method being suitable for the detection of SVOCs in solid waste of the building material type.
The beneficial effects are that:
The invention solves the problems of low extraction efficiency and poor reproducibility of the measurement result of the semi-volatile organic matters in the solid waste sample in the prior art by providing the method for measuring the semi-volatile organic matters in the solid waste, realizes high-efficiency and accurate detection of the semi-volatile organic matters in the solid waste, and reduces the detection limit of morpholine-3, 5-dione and chloromethyl thiocyanate by limiting specific detection conditions.
Detailed Description
The contents of the present invention can be more easily understood by referring to the following detailed description of preferred embodiments of the present invention and examples included. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprising," "including," "having," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified element, step or component. If used in a claim, such phrase will cause the claim to be closed, such that it does not include materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the claim body, rather than immediately following the subject, it is limited to only the elements described in that clause; other elements are not excluded from the stated claims as a whole.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
The singular forms include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or event may or may not occur, and that the description includes both cases where the event occurs and cases where the event does not.
Approximating language, in the specification and claims, may be applied to modify an amount that would not limit the application to the specific amount, but would include an acceptable portion that would be close to the amount without resulting in a change in the basic function involved. Accordingly, the modification of a numerical value with "about", "about" or the like means that the present application is not limited to the precise numerical value. In some examples, the approximating language may correspond to the precision of an instrument for measuring the value. In the description and claims of the application, the range limitations may be combined and/or interchanged, if not otherwise specified, including all the sub-ranges subsumed therein.
Furthermore, the indefinite articles "a" and "an" preceding an element or component of the invention are not limited to the requirements of the number of elements or components (i.e. the number of occurrences). Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component also includes the plural reference unless the amount is obvious to the singular reference.
"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" encompasses the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer". "interpolymer" means a polymer prepared by the polymerization of at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is typically employed to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is typically employed to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing more monomers. "blend" means a polymer formed by the co-mixing of two or more polymers by physical or chemical means.
In order to solve the above problems, a first aspect of the present invention provides a method for determining a semi-volatile organic compound in solid waste, comprising the steps of:
S1, collecting a solid waste sample: collecting solid waste samples by using a clean shovel or a stainless steel device, rapidly collecting the samples into a clean 2mL brown compact bottle, and filling the samples as much as possible; cleaning the outer surface of a sample bottle and a sample adhered by threads, sealing the sample bottle, placing the sample bottle in a refrigerating device at 0-4 ℃ for preservation, and collecting 3 parallel samples from each sample when collecting the samples;
S2, preparing a standard sample: accurately weighing 20mg of target object to be measured in a 25mL clean volumetric flask, and using absolute ethyl alcohol to fix the volume to serve as 5 th-level standard working solution, and gradually diluting the previous-level standard working solution 5 times to obtain the next-level standard working solution until the 1 st-level standard working solution;
S3, pretreating a sample; the weight ratio of the sample to the diatomite is 1: (5-15) mixing, grinding to 120-160 meshes, then adding into an extraction tank, setting the extraction temperature to be 95-120 ℃, setting the extraction pressure to be 1300-1600Pa, setting the extraction time to be 5min, and setting the extraction solvent to be a mixed solution of dichloromethane and acetone, wherein the volume ratio of the dichloromethane to the acetone is 1:1, repeatedly extracting for 3 times to obtain an extracting solution; concentrating the extract to 2mL under reduced pressure by a rotary evaporator, activating by a solid phase extraction device, loading, leaching, eluting, concentrating to 1mL, adding 1 mu L of internal standard, rapidly sealing, and measuring;
S4, placing the pretreated sample and the standard sample into a gas chromatography-mass spectrometer for detection; the gas chromatography mass spectrometer comprises at least a gas chromatography module and a mass spectrometry module.
In some preferred embodiments, the diatomaceous earth in step S3 is diatomaceous earth calcined at a high temperature.
Further preferably, the calcination temperature is 400 to 500 ℃ and the calcination time is 1 to 2 hours.
The invention discovers that the sample SVOCs result reproducibility is good when diatomite calcined at a high temperature of 400-500 ℃ is used for pretreatment of solid waste. The reason is probably that on one hand, the diatomite calcined at high temperature can promote the contact of the solid waste sample and the solvent to a greater extent, and the organic matters to be detected in the sample are fully extracted into the mixed solvent of dichloromethane and acetone; on the other hand, the organic impurities in the diatomite material after high-temperature calcination are removed, the microporous structure of the diatomite is more optimized, the adsorptivity is improved, the loss of the analyte during the extraction is inhibited, and the reproducibility of the measurement and analysis is improved.
In some preferred embodiments, the solid phase extraction device employs a magnesium silicate column.
According to the invention, the combination of rapid solvent extraction and solid phase extraction is adopted in the pretreatment of the sample, so that the semi-volatile organic compounds in the solid waste can be efficiently extracted; when the extraction temperature is set to be 95-120 ℃ and the extraction pressure is set to be 1300-1600Pa, the recovery rate of the target object to be detected can reach more than 85%. The temperature and pressure can be increased to improve the dissolving capacity of the analyte in the solvent on one hand, and on the other hand, the target analyte in the sample can overcome the matrix effect, fully enter the solvent, the resistance of the solvent penetrating into the sample matrix under the specific pressure is weakened, the Van der Waals force and hydrogen bonding between solute molecules and the sample matrix are weakened, the contact between the solvent and the matrix is more sufficient, and the extraction efficiency of the target analyte in the pretreatment process is further promoted.
In some preferred embodiments, the operating conditions of the gas chromatography module in step S4 are: selecting a polysiloxane gas chromatographic column; the temperature of the sample inlet is 290-310 ℃; the sample injection mode is split-flow sample injection; the carrier gas is high-purity helium; the gas chromatographic module adopts temperature programming to separate the target object to be detected.
In some preferred embodiments, the split ratio of the split sample is (3-10): 1.
In some preferred embodiments, the temperature programmed conditions are: keeping at 45 ℃ for 2min; heating to 260 ℃ at a speed of 20 ℃/min for 0min, heating to 280 ℃ at a speed of 6 ℃/min for 0min, and heating to 310 ℃ at 10 ℃/min for 5min.
The invention further finds that when the split ratio of split sample introduction is (3-10): 1, and the temperature programming conditions are set as follows: keeping at 45 ℃ for 2min; heating to 260 ℃ at the speed of 20 ℃/min for 0min, heating to 280 ℃ at the speed of 6 ℃/min for 0min, and heating to 310 ℃ at the speed of 10 ℃/min for 5min, so that the detection limit of morpholine-3, 5-dione and chloromethyl thiocyanate in the solid waste is reduced. The reason is probably that the condition improves the response capability of the gas chromatography-mass spectrometer to the target object to be detected, and reduces the detection limit of SVOCs (especially morpholine-3, 5-dione and chloromethyl thiocyanate) in solid waste.
In some preferred embodiments, the polysiloxane gas chromatography column is Agilent DB-5 30m 0.25mm 0.25 μm.
In some preferred embodiments, the conditions of the mass spectrometry module are: ion source EI, scanning ion range: 35-550amu, ion source temperature 220-240 ℃.
In some preferred embodiments, the internal standard comprises 1, 4-dichlorobenzene-d 4, naphthalene-d 8, acenaphthene-d 10, phenanthrene-d 10,-At least one of d12 and perylene-d 12.
In some preferred embodiments, the target test object comprises bis (2-ethylhexyl) phthalate, phthalimide, 2, 6-bis (trimethylsiloxy) benzoic acid trimethylsilicone ester, dodecamethylcyclohexasiloxane, morpholine-3, 5-dione, aminoacetonitrile, chloromethyl thiocyanate, hexahydro-1, 3, 5-trimethyl-S-triazine, N- ((dimethylamino) methyl) -N-methylformamide, N, N-dimethylurea, trimethylurea, 2-amino-3-hydroxypyridine, 2-chloro-1, 3-thiazole-5-carbaldehyde, tributylamine, N-benzyldiethylamine, 2- (5-amino-3-oxo-3, 6-dihydro-2H-piperazin-1-yl) -acetamide, hexamethylenetetramine, ethyleneglycol bis (2-aminoethylether) tetraacetic acid, acetone dimethylhydrazine, creatinine, N-propyl-2-ylpentyl-4-en-1-amine, 1-methyl-1, 3-diazinon-2, 4-dione, 5-ethyl-2-methyl-4-propylthiazole, propyldichlorophosphine, uric acid, 1, 3-dimethyl-6-semicarbazide, N, N-dimethylpropionamide, diethylenetriamine pentaacetic acid, N, N, N ', N ' -tetramethyl-L-tartaric acid amide, 3' -diaminodipropylamine, glycylsarcosine, at least one of ethylenediamine tetraacetic acid dianhydride, N-dimethyl propenyl urea, 4' -dichloro diphenyl sulfone, 2-acetone bis (1-methyl ethyl) hydrazone, lysergic acid, N-ethyl-2, 3-diketopiperazine and propylimine.
In a second aspect, the invention provides the use of a method for determining semi-volatile organic compounds in solid waste, the method being suitable for the detection of SVOCs in solid waste of the building material type.
In some preferred embodiments, the building material is waste cement.
Examples
Example 1.
The embodiment provides a method for measuring semi-volatile organic compounds in solid waste, which comprises the following steps:
S1, collecting a solid waste sample: collecting solid waste samples by using a clean shovel or a stainless steel device, rapidly collecting the samples into a clean 2mL brown compact bottle, and filling the samples as much as possible; cleaning the outer surface of a sample bottle and a sample adhered by threads, sealing the sample bottle, placing the sample bottle in a refrigerating device at 0-4 ℃ for preservation, and collecting 3 parallel samples from each sample when collecting the samples;
S2, preparing a standard sample: accurately weighing 20mg of target object to be measured in a 25mL clean volumetric flask, and using absolute ethyl alcohol to fix the volume to serve as 5 th-level standard working solution, and gradually diluting the previous-level standard working solution 5 times to obtain the next-level standard working solution until the 1 st-level standard working solution;
S3, pretreating a sample; the weight ratio of the sample to the diatomite is 1:10, grinding to 150 meshes, then adding the mixture into an extraction tank, setting the extraction temperature to be 110 ℃, the extraction pressure to be 1500Pa, the extraction time to be 5min, and the extraction solvent to be a mixed solution of dichloromethane and acetone, wherein the volume ratio of the dichloromethane to the acetone is 1:1, repeatedly extracting for 3 times to obtain an extracting solution; concentrating the extract to 2mL under reduced pressure by a rotary evaporator, activating by a solid phase extraction device, loading, leaching, eluting, concentrating to 1mL, adding 1 mu L of internal standard, rapidly sealing, and measuring;
S4, placing the pretreated sample and the standard sample into a gas chromatography-mass spectrometer for detection; the gas chromatography mass spectrometer comprises a gas chromatography module and a mass spectrometry module.
The diatomite in the step S3 is diatomite calcined at high temperature. The calcination temperature was 450℃and the calcination time was 1.5h.
The solid phase extraction device adopts a magnesium silicate small column.
The working conditions of the gas chromatography module in the step S4 are as follows: selecting a polysiloxane gas chromatographic column; the temperature of the sample inlet is 300 ℃; the sample injection mode is split-flow sample injection; the carrier gas is high-purity helium; the gas chromatographic module adopts temperature programming to separate the target object to be detected.
The split ratio of the split sample injection is 5:1.
The temperature programming conditions are as follows: keeping at 45 ℃ for 2min; heating to 260 ℃ at a speed of 20 ℃/min for 0min, heating to 280 ℃ at a speed of 6 ℃/min for 0min, and heating to 310 ℃ at 10 ℃/min for 5min.
The polysiloxane gas chromatography column was Agilent DB-5 30m 0.25mm 0.25 μm.
The conditions of the mass spectrum module are as follows: ion source EI, scanning ion range: 35-550amu, ion source temperature 230 ℃.
The internal standard is 1, 4-dichlorobenzene-d 4, naphthalene-d 8, acenaphthene-d 10, phenanthrene-d 10,Mixed standard liquid of-d 12 and perylene-d 12, 1, 4-dichlorobenzene-d 4, naphthalene-d 8, acenaphthene-d 10, phenanthrene-d 10,/>The concentrations of both-d 12 and perylene-d 12 were 4000. Mu.g/mL and were purchased from Di-Ma technologies.
The target object to be detected is dimethyl (2-ethylhexyl) phthalate, phthalimide, 2, 6-bis (trimethylsiloxy) benzoic acid trimethylsilicone ester, dodecylcyclohexasiloxane, morpholine-3, 5-dione, aminoacetonitrile, chloromethyl thiocyanate, hexahydro-1, 3, 5-trimethyl-S-triazine, N- ((dimethylamino) methyl) -N-methylformamide, N, N-dimethylurea, trimethyl urea, 2-amino-3-hydroxypyridine, 2-chloro-1, 3-thiazole-5-carbaldehyde, tributylamine, N-benzyldiethylamine, 2- (5-amino-3-oxo-3, 6-dihydro-2H-piperazin-1-yl) -acetamide, hexamethylenetetramine, ethylene glycol bis (2-aminoethylether) tetraacetic acid, acetone dimethylhydrazine, creatinine, N-propyl-2-methylpentyl-4-allyl-1-amine, 1-methyl-1, 3-diazine-2, 4-dione, 2-ethyl-2-aminopropyl-3-hydroxypyridine, 2-chloro-1, 3-thiazole-5-carbaldehyde, tributylamine, N-benzyl-diethylamine, 2- (5-amino-3-oxo-3-2H-piperazin-1-yl) -acetamide, hexamethylenetetramine, ethylene glycol bis (2-aminoethyl ether) tetraacetic acid, acetone dimethylhydrazine, creatinine, N-propyl-2-allyl-4-allyl-1, N-amine, N, N ' -dimethylurea, N-dimethyl-4-carbamide, N-propyl-2-amine, N-propyl-aminopropylenamide, N-3-methyl-3 ' -aminopropylenamide, N, N-methyl-3-propyl-methyl-N-propyl-2-amine, N ' -methyl-N-propyl-methyl-N-methyl-2-methyl-N-methyl ether, 4,4' -dichlorodiphenyl sulfone, 2-acetonebis (1-methylethyl) hydrazone, lysergic acid, N-ethyl-2, 3-diketopiperazine, propylimine.
The solid waste sample was waste cement with a sampling amount of 10g.
Example 2.
A method for measuring volatile organic compounds in solid waste is described in example 1. Except that the diatomaceous earth was not calcined at high temperature.
Example 3.
A method for measuring volatile organic compounds in solid waste is described in example 1. The difference is that the calcination temperature was 600℃and the calcination time was 1h.
Example 4.
A method for measuring volatile organic compounds in solid waste is described in example 1. The difference is that the extraction solvent is a mixed solution of n-hexane and acetone, and the volume ratio of the n-hexane to the acetone is 1:1.
Example 5.
A method for measuring volatile organic compounds in solid waste is described in example 1. Except that the polysiloxane gas chromatography column was Agilent DB-5 10 m.times.0.1 mm.times.0.1. Mu.m.
Example 6.
A method for measuring volatile organic compounds in solid waste is described in example 1. The difference is that the split ratio is 15:1.
Example 7.
A method for measuring volatile organic compounds in solid waste is described in example 1. The difference is that the temperature programming conditions are as follows: keeping at 45 ℃ for 2min; heating to 260 ℃ at a speed of 25 ℃ per minute for 0min, heating to 280 ℃ at a speed of 5 ℃ per minute for 0min, and heating to 310 ℃ at 15 ℃ per minute for 5min.
Performance test method
Results precision:
And (3) respectively placing the same sample into 3 headspace bottles for pretreatment during sampling, carrying out on-machine measurement corresponding to the conditions of each embodiment, and recording the relative standard deviation of the sum of the measured concentrations of the target substances to be measured in the sample measurement result.
Detection limit:
Diatomaceous earth was used as a blank sample, and pretreatment and on-machine detection were performed as in examples 1 to 7. The detection limit of morpholine-3, 5-dione and chloromethyl thiocyanate was calculated from the detection limit = 3-fold standard deviation of the blank.
Performance test data
Finally, it is pointed out that the foregoing examples are illustrative only and serve to explain some of the features of the method according to the invention. The appended claims are intended to claim the broadest possible scope and the embodiments presented herein are merely illustrative of selected implementations based on combinations of all possible embodiments. It is, therefore, not the intention of the applicant that the appended claims be limited by the choice of examples illustrating the features of the invention. Some numerical ranges used in the claims also include sub-ranges within which variations in these ranges should also be construed as being covered by the appended claims where possible.
Claims (2)
1. A method for determining semi-volatile organic compounds in solid waste, comprising the steps of:
S1, collecting a solid waste sample: collecting solid waste samples by using a clean shovel or a stainless steel device, rapidly collecting the samples into a clean 2mL brown compact bottle, and filling the samples as much as possible; cleaning the outer surface of a sample bottle and a sample adhered by threads, sealing the sample bottle, placing the sample bottle in a refrigerating device at 0-4 ℃ for preservation, and collecting 3 parallel samples from each sample when collecting the samples;
S2, preparing a standard sample: accurately weighing 20mg of target object to be measured in a 25mL clean volumetric flask, and using absolute ethyl alcohol to fix the volume to serve as 5 th-level standard working solution, and gradually diluting the previous-level standard working solution 5 times to obtain the next-level standard working solution until the 1 st-level standard working solution;
S3, pretreating a sample; the weight ratio of the sample to the diatomite is 1:10, grinding to 150 meshes, then adding the mixture into an extraction tank, setting the extraction temperature to be 110 ℃, the extraction pressure to be 1500Pa, the extraction time to be 5min, and the extraction solvent to be a mixed solution of dichloromethane and acetone, wherein the volume ratio of the dichloromethane to the acetone is 1:1, repeatedly extracting for 3 times to obtain an extracting solution; concentrating the extract to 2mL under reduced pressure by a rotary evaporator, activating by a solid phase extraction device, loading, leaching, eluting, concentrating to 1mL, adding 1 mu L of internal standard, rapidly sealing, and measuring;
s4, placing the pretreated sample and the standard sample into a gas chromatography-mass spectrometer for detection; the gas chromatography mass spectrometer comprises a gas chromatography module and a mass spectrometry module;
the diatomite in the step S3 is diatomite subjected to high-temperature calcination; the calcination temperature is 450 ℃, and the calcination time is 1.5h;
the solid phase extraction device adopts a magnesium silicate small column;
the working conditions of the gas chromatography module in the step S4 are as follows: selecting a polysiloxane gas chromatographic column; the temperature of the sample inlet is 300 ℃; the sample injection mode is split-flow sample injection; the carrier gas is high-purity helium; the gas chromatographic module adopts temperature programming to separate a target object to be detected;
The split ratio of the split sample injection is 5:1, a step of;
The temperature programming conditions are as follows: keeping at 45 ℃ for 2min; heating to 260 ℃ at a speed of 20 ℃/min for 0min, heating to 280 ℃ at a speed of 6 ℃/min for 0min, and heating to 310 ℃ at a speed of 10 ℃/min for 5min;
The polysiloxane gas chromatographic column is Agilent DB-5 30m multiplied by 0.25mm multiplied by 0.25 mu m;
the conditions of the mass spectrum module are as follows: ion source EI, scanning ion range: 35-550amu, ion source temperature 230 ℃;
The internal standard is 1, 4-dichlorobenzene-d 4, naphthalene-d 8, acenaphthene-d 10, phenanthrene-d 10, Mixed standard liquid of-d 12 and perylene-d 12, 1, 4-dichlorobenzene-d 4, naphthalene-d 8, acenaphthene-d 10, phenanthrene-d 10,/>The concentrations of both d12 and perylene-d 12 were 4000. Mu.g/mL, purchased from Di-Ma technologies;
The target object to be detected is dimethyl (2-ethylhexyl) phthalate, phthalimide, 2, 6-bis (trimethylsiloxy) benzoic acid trimethylsilicone ester, dodecylcyclohexasiloxane, morpholine-3, 5-dione, aminoacetonitrile, chloromethyl thiocyanate, hexahydro-1, 3, 5-trimethyl-S-triazine, N- ((dimethylamino) methyl) -N-methylformamide, N, N-dimethylurea, trimethyl urea, 2-amino-3-hydroxypyridine, 2-chloro-1, 3-thiazole-5-carbaldehyde, tributylamine, N-benzyldiethylamine, 2- (5-amino-3-oxo-3, 6-dihydro-2H-piperazin-1-yl) -acetamide, hexamethylenetetramine, ethylene glycol bis (2-aminoethylether) tetraacetic acid, acetone dimethylhydrazine, creatinine, N-propyl-2-methylpentyl-4-allyl-1-amine, 1-methyl-1, 3-diazine-2, 4-dione, 2-ethyl-2-aminopropyl-3-hydroxypyridine, 2-chloro-1, 3-thiazole-5-carbaldehyde, tributylamine, N-benzyl-diethylamine, 2- (5-amino-3-oxo-3-2H-piperazin-1-yl) -acetamide, hexamethylenetetramine, ethylene glycol bis (2-aminoethyl ether) tetraacetic acid, acetone dimethylhydrazine, creatinine, N-propyl-2-allyl-4-allyl-1, N-amine, N, N ' -dimethylurea, N-dimethyl-4-carbamide, N-propyl-2-amine, N-propyl-aminopropylenamide, N-3-methyl-3 ' -aminopropylenamide, N, N-methyl-3-propyl-methyl-N-propyl-2-amine, N ' -methyl-N-propyl-methyl-N-methyl-2-methyl-N-methyl ether, 4,4' -dichlorodiphenyl sulfone, 2-acetonebis (1-methylethyl) hydrazone, lysergic acid, N-ethyl-2, 3-diketopiperazine and propylimine;
the solid waste sample was waste cement with a sampling amount of 10g.
2. Use of the method for determining the amount of semi-volatile organic compounds in solid waste according to claim 1, characterized in that the method is suitable for the detection of SVOCs in solid waste of the building material type.
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