CN112666288A - Method for measuring volatile organic compounds in solid waste - Google Patents
Method for measuring volatile organic compounds in solid waste Download PDFInfo
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- CN112666288A CN112666288A CN202011529748.2A CN202011529748A CN112666288A CN 112666288 A CN112666288 A CN 112666288A CN 202011529748 A CN202011529748 A CN 202011529748A CN 112666288 A CN112666288 A CN 112666288A
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- solid waste
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- 238000000034 method Methods 0.000 title claims abstract description 57
- 239000002910 solid waste Substances 0.000 title claims abstract description 53
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 43
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001514 detection method Methods 0.000 claims abstract description 28
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005065 mining Methods 0.000 claims abstract description 8
- 239000002699 waste material Substances 0.000 claims abstract description 6
- 238000007781 pre-processing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000004817 gas chromatography Methods 0.000 claims description 14
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000005350 fused silica glass Substances 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical compound CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 8
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 claims description 8
- CNPVJWYWYZMPDS-UHFFFAOYSA-N 2-methyldecane Chemical compound CCCCCCCCC(C)C CNPVJWYWYZMPDS-UHFFFAOYSA-N 0.000 claims description 8
- GXDHCNNESPLIKD-UHFFFAOYSA-N 2-methylhexane Chemical compound CCCCC(C)C GXDHCNNESPLIKD-UHFFFAOYSA-N 0.000 claims description 8
- PFEOZHBOMNWTJB-UHFFFAOYSA-N 3-methylpentane Chemical compound CCC(C)CC PFEOZHBOMNWTJB-UHFFFAOYSA-N 0.000 claims description 8
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims description 8
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 8
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 8
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 claims description 8
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- OCJBOOLMMGQPQU-RHQRLBAQSA-N 1,4-dichloro-2,3,5,6-tetradeuteriobenzene Chemical compound [2H]C1=C([2H])C(Cl)=C([2H])C([2H])=C1Cl OCJBOOLMMGQPQU-RHQRLBAQSA-N 0.000 claims description 7
- MVPPADPHJFYWMZ-RALIUCGRSA-N 1-chloro-2,3,4,5,6-pentadeuteriobenzene Chemical compound [2H]C1=C([2H])C([2H])=C(Cl)C([2H])=C1[2H] MVPPADPHJFYWMZ-RALIUCGRSA-N 0.000 claims description 7
- 238000001819 mass spectrum Methods 0.000 claims description 7
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 claims description 7
- XHNIFDXYGLPJLP-UHFFFAOYSA-N 2,4,6-trimethyl-Octane Chemical compound CCC(C)CC(C)CC(C)C XHNIFDXYGLPJLP-UHFFFAOYSA-N 0.000 claims description 6
- HDGQICNBXPAKLR-UHFFFAOYSA-N 2,4-dimethylhexane Chemical compound CCC(C)CC(C)C HDGQICNBXPAKLR-UHFFFAOYSA-N 0.000 claims description 6
- FONXOARHSFUBAN-UHFFFAOYSA-N 2,6,11-trimethyldodecane Chemical compound CC(C)CCCCC(C)CCCC(C)C FONXOARHSFUBAN-UHFFFAOYSA-N 0.000 claims description 6
- JJRUZTXRDDMYGM-UHFFFAOYSA-N 3-Methyldecane Chemical compound CCCCCCCC(C)CC JJRUZTXRDDMYGM-UHFFFAOYSA-N 0.000 claims description 6
- VLJXXKKOSFGPHI-UHFFFAOYSA-N 3-methylhexane Chemical compound CCCC(C)CC VLJXXKKOSFGPHI-UHFFFAOYSA-N 0.000 claims description 6
- DOGIHOCMZJUJNR-UHFFFAOYSA-N 4-methyloctane Chemical compound CCCCC(C)CCC DOGIHOCMZJUJNR-UHFFFAOYSA-N 0.000 claims description 6
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- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 6
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- 239000012159 carrier gas Substances 0.000 claims description 5
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
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- 229940078552 o-xylene Drugs 0.000 claims description 5
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 4
- XTIADNINQBIUNR-UHFFFAOYSA-N 2,3,5,8-tetramethyldecane Chemical compound CCC(C)CCC(C)CC(C)C(C)C XTIADNINQBIUNR-UHFFFAOYSA-N 0.000 claims description 4
- YKPNYFKOKKKGNM-UHFFFAOYSA-N 2,3,5-trimethylheptane Chemical compound CCC(C)CC(C)C(C)C YKPNYFKOKKKGNM-UHFFFAOYSA-N 0.000 claims description 4
- ZCTGYLNFWOQVHV-UHFFFAOYSA-N 2,3-dimethyldecane Chemical compound CCCCCCCC(C)C(C)C ZCTGYLNFWOQVHV-UHFFFAOYSA-N 0.000 claims description 4
- SWDJLVOSNCGQGB-UHFFFAOYSA-N 2,6,8-trimethyldecane Chemical compound CCC(C)CC(C)CCCC(C)C SWDJLVOSNCGQGB-UHFFFAOYSA-N 0.000 claims description 4
- NRJUFUBKIFIKFI-UHFFFAOYSA-N 4-ethyloctane Chemical compound CCCCC(CC)CCC NRJUFUBKIFIKFI-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
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- NEZRFXZYPAIZAD-UHFFFAOYSA-N ethylcyclobutane Chemical compound CCC1CCC1 NEZRFXZYPAIZAD-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
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- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 4
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 claims description 4
- JCJGCZBSINPZAJ-UHFFFAOYSA-N 2,7,10-trimethyldodecane Chemical compound CCC(C)CCC(C)CCCCC(C)C JCJGCZBSINPZAJ-UHFFFAOYSA-N 0.000 claims description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 3
- BSPCSKHALVHRSR-UHFFFAOYSA-N 2-chlorobutane Chemical compound CCC(C)Cl BSPCSKHALVHRSR-UHFFFAOYSA-N 0.000 claims description 3
- ILUAAIDVFMVTAU-UHFFFAOYSA-N cyclohex-4-ene-1,2-dicarboxylic acid Chemical compound OC(=O)C1CC=CCC1C(O)=O ILUAAIDVFMVTAU-UHFFFAOYSA-N 0.000 claims description 3
- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 claims description 3
- ULYZAYCEDJDHCC-UHFFFAOYSA-N isopropyl chloride Chemical compound CC(C)Cl ULYZAYCEDJDHCC-UHFFFAOYSA-N 0.000 claims description 3
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- GWEDODYYNURODY-UHFFFAOYSA-N 1-[ethoxy(methylsulfanyl)phosphoryl]oxyethane Chemical compound CCOP(=O)(SC)OCC GWEDODYYNURODY-UHFFFAOYSA-N 0.000 claims description 2
- -1 2-dimethyldecane Chemical compound 0.000 claims description 2
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- QTWKINKGAHTPFJ-UHFFFAOYSA-N 2-(butan-2-yldisulfanyl)butane Chemical compound CCC(C)SSC(C)CC QTWKINKGAHTPFJ-UHFFFAOYSA-N 0.000 description 2
- GTJOHISYCKPIMT-UHFFFAOYSA-N 2-methylundecane Chemical compound CCCCCCCCCC(C)C GTJOHISYCKPIMT-UHFFFAOYSA-N 0.000 description 2
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of detection, in particular to a method for determining 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, preprocessing a sample; and S4, placing the pretreated sample and the standard sample into a headspace-gas chromatography-mass spectrometer for detection. The invention provides a method for determining volatile organic compounds in solid waste, which is applied to detection of VOCs in mining waste slag solid waste. The method can be used for rapidly and efficiently detecting dozens of target compounds, has good detection reproducibility on low-concentration samples, and simultaneously reduces the detection limit of toluene and hexamethyldisiloxane.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for determining volatile organic compounds in solid waste and application thereof.
Background
Volatile Organic Compounds (vollate Organic Compounds) generally refer to Organic Compounds having a boiling point in the range of 50 to 260 ℃ and a saturated vapor pressure in excess of 133.132kPa at room temperature. With the acceleration of urbanization process and the increasing improvement of living standard of residents in China, the demand of corresponding resources is increased year by year, so that the total amount and the types of solid wastes are in an increasing trend. Because the solid waste has the characteristics of large yield, dispersed sources, complex components, variable shapes and properties and the like, the solid waste not only occupies a large amount of land and space resources in the stacking process, but also causes harmful substances to enter water, soil and atmosphere through rainwater washing and surface runoff, thereby seriously damaging the original ecological structure. Meanwhile, the solid waste releases volatile and semi-volatile organic pollutants due to exposure to the sun, so that the hidden danger that the ecological environment is seriously damaged and the daily life of residents is influenced due to secondary pollution caused by chemical reaction caused by improper treatment mode exists. From the economic development condition and the pollution trend of China at present, the monitoring of organic pollutants in solid waste is bound to become an important target of environmental monitoring.
The VOCs in the solid waste comprise scavengeable hydrocarbons, benzene series, volatile organic compounds, volatile petroleum hydrocarbons and the like, and are mainly derived from the combustion of fuels such as gasoline, wood, coal, natural gas and the like, solvents, paints, glues and other products applied to families and workplaces. However, VOCs destroy the ozone layer, easily cause chemical smog, and can also be combined with fine dust particles in dust to form fog, which brings negative effects on the lung of a human body and the health of various organisms such as animals and plants, has the harm of teratogenesis, mutagenesis, carcinogenesis and the like to the human body, and the VOCs continuously migrate in environmental media such as soil, water, atmosphere and the like through the processes of leaching, volatilization, sedimentation and the like, and finally form accumulation in soil and solid waste.
The solid waste has the characteristics of low content of VOCs, high volatility and high matrix interference, and a Soxhlet extraction method is usually adopted to extract a sample in the traditional detection process. Although the Soxhlet extraction method has simple equipment and good extraction efficiency, the method consumes more organic solvent, has long extraction time, and easily extracts sulfur from the matrix during extraction to cause negative influence on the instrument. The static headspace method is characterized in that a sample is added into a constant-temperature closed space of a headspace bottle, volatile components in the sample volatilize to the headspace of a container to generate vapor pressure, and when a gas phase and a liquid phase reach thermodynamic dynamic equilibrium, a gas phase sample is taken for chromatographic analysis. The existing research finds that the method effectively simplifies the sample pretreatment time, does not need an extraction solvent, and inhibits the loss of VOCs to be detected in solid waste, but the method has poor reproducibility and low sensitivity of detection and analysis. Based on this, the research of a detection method for efficiently and accurately detecting VOCs in solid waste becomes an urgent problem to be solved in the field.
Disclosure of Invention
The invention provides a method for measuring volatile organic compounds in solid waste, overcomes the defect of poor separation degree of xylene isomers in the prior art, and realizes the technical effect of efficiently and accurately detecting VOCs in the solid waste.
The invention provides a method for measuring volatile organic compounds in solid waste, which comprises the following steps:
s1, collecting a solid waste sample;
s2, preparing a standard sample;
s3, preprocessing a sample;
s4, placing the pretreated sample and the standard sample into a headspace-gas chromatography-mass spectrometer for detection; the headspace-gas chromatography-mass spectrometer at least comprises a headspace sampler module, a gas chromatography module and a mass spectrum module.
In a preferred embodiment, the operating conditions of the headspace sampler module in step S4 are: the heating balance temperature is 82-88 ℃, the balance time is 20-30min, the sampling needle temperature is 88-92 ℃, the transmission line temperature is 100-.
In a preferred embodiment, the operating conditions of the gas chromatography module are: selecting a fused quartz capillary column as a chromatographic column; the temperature of the sample inlet is 210-; the carrier gas is high-purity helium; and the gas chromatography module adopts programmed temperature rise to separate the target object to be detected.
In a preferred embodiment, the split ratio of the split feed is (25-35): 1.
in a preferred embodiment, the temperature programming is specifically configured to: keeping at 45 deg.C for 2min, heating to 120 deg.C at 10 deg.C/min for 0min, and heating to 220 deg.C at 15 deg.C/min for 0 min.
In a preferred embodiment, the operating conditions of the mass spectrometry module are: the scanning ion range of the ion source EI is 30-270amu, and the ion source temperature is 280-350 ℃.
In a preferred embodiment, the internal standard in the step S3 is at least one of chlorobenzene-d 5, 1, 4-dichlorobenzene-d 4 and fluorobenzene.
In a preferred embodiment, the fused silica capillary column is Agilent DB-VRX 30m x 0.25mm x 1.4 μm.
In a preferred embodiment, the target analyte includes dichloromethane, trimethylsilanol, 2-methylpentane, 3-methylpentane, n-hexane, 1-ethylcyclobutane, 1, 2-dichloroethane, 2-methylhexane, benzene, hexamethyldisiloxane, heptane, cyclohexane, dimethyldisulfide, sec-butyl acetate, toluene, butyl acetate, chlorobenzene, ethylbenzene, m-xylene, p-xylene, styrene, n-decane, 2,7, 7-tetramethyloctane, 2-ethylhexanol, tridecane, 2,3, 5-trimethylheptane, 2,6, 8-trimethyldecane, 2,3,5, 8-tetramethyldecane, 2, 6-dimethyldecane, 4-ethyloctane, 2, 3-dimethyldecane, o-decylhydroxylamine, dimethyldecane, dimethyldecan, dimethyl, 2-methyl decane, acetone, ethanethiol, dimethyl sulfide, 1-chloropropane, 2-chloropropane, 3-chloropropane, 2-butanone, 2-chlorobutane, methyl cyclopentane, methanesulfonic acid, 3-methyl hexane, 2,4, 6-trimethyl octane, 2, 4-dimethyl hexane, 2,6, 11-trimethyl dodecane, 2,7, 10-trimethyl dodecane, 3-methyl decane, 4-methyl octane, diethyl methyl thiophosphate, o-xylene, triethyl thiophosphate, cis-4-cyclohexene-1, 2-dicarboxylic acid, and diethyl phosphite.
The invention provides an application of a method for determining volatile organic compounds in solid waste, which is applied to detection of VOCs in solid waste such as mining waste residues.
Has the advantages that:
the invention provides a method for determining volatile organic compounds in solid waste, which is applied to detection of VOCs in mining waste residue solid waste. The method can be used for rapidly and efficiently detecting dozens of target compounds, has good detection reproducibility on low-concentration samples, and simultaneously reduces the detection limit of toluene and hexamethyldisiloxane.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. 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, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, 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, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range 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 a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" embraces the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer". "interpolymer" means a polymer prepared by polymerizing at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is generally used to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is generally used to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing more monomers. "blend" means a polymer formed by two or more polymers being mixed together by physical or chemical means.
In order to solve the above problems, a first aspect of the present invention provides a method for measuring volatile organic compounds in solid waste, comprising the steps of:
s1, collecting a solid waste sample: collecting a solid waste sample using a clean metal sampling tool, collecting the sample in a clean 2mL brown compact bottle and filling; removing the sample adhered to the threads and the outer surface of the sample bottle, sealing the sample bottle, and storing in a refrigeration device at 0-4 ℃ to obtain a sample to be detected; all samples were collected in 3 replicates;
s2, preparing a standard sample: accurately weighing 20mg of target object to be measured in a 25mL clean volumetric flask, using absolute ethyl alcohol for constant volume to serve as 5-level standard working solution, diluting the previous-level standard working solution by 5 times step by step to obtain the next-level standard working solution till the 1 st-level standard working solution;
s3, pretreatment of a sample: taking out a sample to be detected, weighing 2g of the sample in a clean headspace bottle after the sample is recovered to the room temperature, adding 10mL of Milli-Q ultrapure water and 2 muL of internal standard into the headspace bottle, sealing, oscillating for 5-10min at the frequency of 120-;
s4, placing the pretreated sample and the standard sample into a headspace-gas chromatography-mass spectrometer for detection; the headspace-gas chromatography-mass spectrometer at least comprises a headspace sampler module, a gas chromatography module and a mass spectrum module.
The combination of the headspace sampling system and the gas chromatography-mass spectrometry is an effective method for detecting volatile organic compounds in the solid waste sample, and the method can accelerate and simplify the sample pretreatment steps and improve the analysis efficiency. The headspace-gas analysis is characterized in that the chromatographic analysis is carried out on the upper air-gas phase part of the sample matrix under the equilibrium state, so that the analysis defect that the interference of the co-extract cannot be stripped in the solid-phase and liquid-phase extraction methods is overcome, and the interference of the sample matrix on the analysis and detection is obviously reduced by the method.
In some preferred embodiments, the operating conditions of the headspace sampler module in step S4 are: the heating balance temperature is 82-88 ℃, the balance time is 20-30min, the sampling needle temperature is 88-92 ℃, the transmission line temperature is 100-.
The invention finds that the higher the heating balance temperature of the headspace sample injector is and the longer the balance time is, the better the sample measuring effect is, and when the temperature is too high and the time is too long, the pressure of the headspace gas rises, the pressure resistance and the air tightness decline, and the peak area response is not stable enough, and the repeatability of quantitative detection declines. When the heating balance temperature is 82-88 ℃ and the balance time is 20-30min, the detection effect is better.
Further preferably, the heating equilibrium temperature is 85 ℃ and the equilibrium time is 25 min.
In some preferred embodiments, the operating conditions of the gas chromatography module are: selecting a fused quartz capillary column as a chromatographic column; the temperature of the sample inlet is 210-; the carrier gas is high-purity helium; and the gas chromatography module adopts programmed temperature rise to separate the target object to be detected.
In some preferred embodiments, the split ratio of the split feed is (25-35): 1.
the split ratio is (split flow rate + column volume flow rate)/column volume flow rate. The measurement effect is directly influenced by the size of the sample amount of the chromatogram, the problems of too wide chromatographic peak, small separation degree and poor quantitative result easily occur when the sample amount is too large, and higher requirements are provided for the sensitivity of an instrument detector when the sample amount is too small, and a target object to be measured is not easily detected; the selection of split-flow sample injection is an effective method for protecting the capillary chromatographic column and giving consideration to both the analysis sensitivity and the good peak appearance. The invention discovers that the selected split ratio is (25-35): 1, the combined action of specific gas chromatography and mass spectrum conditions can improve the uniform vaporization of sample composition molecules, improve the split flow discrimination phenomenon and improve the accuracy of quantitative analysis.
In some preferred embodiments, the temperature programming is specifically configured to: keeping at 45 deg.C for 2min, heating to 120 deg.C at 10 deg.C/min for 0min, and heating to 220 deg.C at 15 deg.C/min for 0 min.
In some preferred embodiments, the operating conditions of the mass spectrometry module are: the scanning ion range of the ion source EI is 30-270amu, and the ion source temperature is 280-350 ℃.
In some preferred embodiments, the internal standard in the S3 step is at least one of chlorobenzene-d 5(CAS number 3114-55-4), 1, 4-dichlorobenzene-d 4(CAS number 3855-82-1), fluorobenzene (CAS number 462-06-6).
In some preferred embodiments, the fused silica capillary column is Agilent DB-VRX 30m by 0.25mm by 1.4 μm.
In some preferred embodiments, the target analyte includes, but is not limited to, methylene chloride, trimethylsilanol, 2-methylpentane, 3-methylpentane, n-hexane, 1-ethylcyclobutane, 1, 2-dichloroethane, 2-methylhexane, benzene, hexamethyldisiloxane, heptane, cyclohexane, dimethyldisulfide, sec-butyl acetate, toluene, butyl acetate, chlorobenzene, ethylbenzene, m-xylene, p-xylene, styrene, n-decane, 2,7, 7-tetramethyloctane, 2-ethylhexanol, tridecane, 2,3, 5-trimethylheptane, 2,6, 8-trimethyldecane, 2,3,5, 8-tetramethyldecane, 2, 6-dimethyldecane, 4-ethyloctane, 2, 3-dimethyldecane, o-decylhydroxylamine, ethyl-dimethyldecane, 3-dimethyldecane, sec-butyldisulfide, toluene, butyl acetate, 2-methyldecane, acetone, ethanethiol, dimethylsulfide, 1-chloropropane, 2-chloropropane, 3-chloropropane, 2-butanone, 2-chlorobutane, methylcyclopentane, methanesulfonic acid, 3-methylhexane, 2,4, 6-trimethyloctane, 2, 4-dimethylhexane, 2,6, 11-trimethyldodecane, 2,7, 10-trimethyldodecane, 3-methyldecane, 4-methyloctane, diethyl methylthiophosphate, o-xylene, triethylthiophosphate, cis-4-cyclohexene-1, 2-dicarboxylic acid, and diethyl phosphite.
Still further preferably, the split ratio of the split sample injection is 30: 1.
the invention finds that when the shunt ratio is set to be 30: 1, the problem that part of xylene isomers cannot be separated is solved; the method can separate the peak time of o-xylene and m/p-xylene to about 30 s. On one hand, the arrangement of the condition avoids that the main component is overloaded to generate a flat top peak, or the main peak is swallowed to form a small area peak to cause poor separation degree, so that an error is generated on a detection result, and on the other hand, the negative influence brought by impurities in the sample injection process is reduced near the larger main peak of the carrier gas flow; the invention also discovers that when the split ratio is 30: on the premise of 1, the headspace conditions are set as follows: the heating equilibrium temperature is 82-88 ℃, the equilibrium time is 20-30min, and the detection limit of the toluene and hexamethyldisiloxane is reduced under the specific conditions of gas chromatography and mass spectrum; the reasons may be that the intermolecular forces between the target organic substance and the solid waste matrix are weakened under the conditions, the activation energy required for the resolution process is reduced, and the detection limit of the instrument for toluene and hexamethyldisiloxane is reduced.
The invention provides an application of a method for determining volatile organic compounds in solid waste, which is applied to detection of VOCs in solid waste such as mining waste residues.
In some preferred embodiments, the mining slag is limestone mining slag.
Examples
Example 1.
The embodiment provides a method for measuring volatile organic compounds in solid waste, which comprises the following steps:
s1, collecting a solid waste sample: collecting a solid waste sample using a clean metal sampling tool, collecting the sample in a clean 2mL brown compact bottle and filling; removing the threads of the sample bottle and samples adhered to the outer surface of the sample bottle, sealing the sample bottle, and storing in a refrigeration device at 0 ℃ to obtain samples to be detected, wherein 3 parallel samples are collected from all the samples;
s2, preparing a standard sample: accurately weighing 20mg of target object to be measured in a 25mL clean volumetric flask, using absolute ethyl alcohol for constant volume to serve as 5-level standard working solution, diluting the previous-level standard working solution by 5 times step by step to obtain the next-level standard working solution till the 1 st-level standard working solution;
s3, pretreatment of a sample: taking out a sample to be detected, placing the sample for 10h at 26 ℃, then weighing 2g of the sample in a clean headspace bottle, adding 10mL of Milli-Q ultrapure water and 2 muL of internal standard into the headspace bottle, sealing, oscillating for 10min at the frequency of 150 times/min, and preparing to be detected;
s4, placing the pretreated sample and the standard sample into a headspace-gas chromatography-mass spectrometer for detection; the headspace-gas chromatography-mass spectrometer comprises a headspace sampler module, a gas chromatography module and a mass spectrum module.
The operating conditions of the headspace sampler module in step S4 are: the heating balance temperature is 85 ℃, the balance time is 25min, the temperature of the sampling needle is 90 ℃, the temperature of the transmission line is 100 ℃, and the sampling volume is 0.8 mL.
The working conditions of the gas chromatography module are as follows: selecting a fused quartz capillary column as a chromatographic column; the temperature of the sample inlet is 220 ℃, the pressure of the sample inlet is 1500psi, and the sample introduction mode is split stream sample introduction; the carrier gas is high-purity helium; and the gas chromatography module adopts programmed temperature rise to separate the target object to be detected.
The split ratio of split sample injection is 30: 1.
the temperature programming is specifically set as follows: keeping at 45 deg.C for 2min, heating to 120 deg.C at 10 deg.C/min for 0min, and heating to 220 deg.C at 15 deg.C/min for 0 min.
The working conditions of the mass spectrum module are as follows: the scanning ion range of the ion source EI is 30-270amu, and the ion source temperature is 300 ℃.
The internal standard in the step S3 is a mixed internal standard solution of chlorobenzene-d 5(CAS number 3114-55-4), 1, 4-dichlorobenzene-d 4(CAS number 3855-82-1) and fluorobenzene (CAS number 462-06-6), which is purchased from Shanghai' an spectral analysis science and technology Limited company with a product number of CDGG-120004-02, and the concentrations of chlorobenzene-d 5, 1, 4-dichlorobenzene-d 4 and fluorobenzene in the mixed internal standard solution are all 2000 mg/L.
The fused silica capillary column is Agilent DB-VRX 30m multiplied by 0.25mm multiplied by 1.4 mu m.
The target object to be detected is dichloromethane, trimethylsilanol, 2-methylpentane, 3-methylpentane, n-hexane, 1-ethylcyclobutane, 1, 2-dichloroethane, 2-methylhexane, benzene, hexamethyldisiloxane, heptane, cyclohexane, dimethyl disulfide, sec-butyl acetate, toluene, butyl acetate, chlorobenzene, ethylbenzene, m-xylene, p-xylene, o-xylene, styrene, n-decane, 2,7, 7-tetramethyloctane, 2-ethylhexanol, tridecane, 2,3, 5-trimethylheptane, 2,6, 8-trimethyldecane, 2,3,5, 8-tetramethyldecane, 2, 6-dimethyldecane, 4-ethyloctane, 2, 3-dimethyldecane, o-decylhydroxylamine, 2-methyldecane.
The solid waste sample is limestone mining waste residue.
Example 2.
The specific implementation mode of the method for measuring the volatile organic compounds in the solid waste is the same as that of example 1. The difference lies in that the flow dividing ratio is 25: 1.
example 3.
The specific implementation mode of the method for measuring the volatile organic compounds in the solid waste is the same as that of example 1. The difference lies in that the flow dividing ratio is 35: 1.
example 3.
The specific implementation mode of the method for measuring the volatile organic compounds in the solid waste is the same as that of example 1. The difference lies in that the flow dividing ratio is 10: 1.
example 4.
The specific implementation mode of the method for measuring the volatile organic compounds in the solid waste is the same as that of example 1. The difference is that the heating equilibrium temperature is 75 ℃, and the equilibrium time is 30 min.
Example 5.
The specific implementation mode of the method for measuring the volatile organic compounds in the solid waste is the same as that of example 1. The difference is that the heating equilibrium temperature is 95 ℃, and the equilibrium time is 20 min.
Example 6.
The specific implementation mode of the method for measuring the volatile organic compounds in the solid waste is the same as that of example 1. The different points are that the temperature programming is specifically set as follows: keeping at 45 deg.C for 2min, increasing the temperature to 120 deg.C for 0min at 12 deg.C/min, and increasing the temperature to 220 deg.C for 0min at 15 deg.C/min.
Example 7.
The specific implementation mode of the method for measuring the volatile organic compounds in the solid waste is the same as that of example 1. The difference is that the fused silica capillary column is Agilent DB-VRX 30m x 0.45mm x 1.8 μm.
Performance test method
Separation of xylene isomers:
the difference between the retention times of ortho-xylene and para/meta-xylene was calculated, and the larger the difference between the retention times, the better the separation.
Reproducibility of results:
when in sampling, the same sample is respectively put into 3 headspace bottles for pretreatment, the on-machine determination is carried out corresponding to the conditions of each embodiment, and the RSD of the sum of the mass concentration of the target substance to be detected in the sample measurement result is recorded.
Detection limits of toluene, hexamethyldisiloxane:
2g of the burned GF/F film was used as a blank and examined by the methods of examples 1 to 7. The detection limit of toluene and hexamethyldisiloxane was calculated from the detection limit of 3 blank standard deviations.
Performance test data
Finally, it is pointed out that the foregoing examples are illustrative only, serving to explain some of the characteristics of the process according to the invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. A method for measuring volatile organic compounds in solid waste is characterized by comprising the following steps:
s1, collecting a solid waste sample;
s2, preparing a standard sample;
s3, preprocessing a sample;
s4, placing the pretreated sample and the standard sample into a headspace-gas chromatography-mass spectrometer for detection; the headspace-gas chromatography-mass spectrometer at least comprises a headspace sampler module, a gas chromatography module and a mass spectrum module.
2. The method of claim 1, wherein the headspace sampler module in step S4 is operated under the following conditions: the heating balance temperature is 82-88 ℃, the balance time is 20-30min, the sampling needle temperature is 88-92 ℃, the transmission line temperature is 100-.
3. The method for measuring volatile organic compounds in solid waste according to claim 1, wherein the operating conditions of the gas chromatography module are as follows: selecting a fused quartz capillary column as a chromatographic column; the temperature of the sample inlet is 210-; the carrier gas is high-purity helium; and the gas chromatography module adopts programmed temperature rise to separate the target object to be detected.
4. The method for determining volatile organic compounds in solid waste according to claim 3, wherein the split injection has a split ratio of (25-35): 1.
5. the method for measuring volatile organic compounds in solid waste according to claim 3, wherein the temperature programming is specifically configured to: keeping at 45 deg.C for 2min, heating to 120 deg.C at 10 deg.C/min for 0min, and heating to 220 deg.C at 15 deg.C/min for 0 min.
6. The method for measuring volatile organic compounds in solid waste according to claim 1, wherein the operating conditions of the mass spectrometry module are as follows: the scanning ion range of the ion source EI is 30-270amu, and the ion source temperature is 280-350 ℃.
7. The method for measuring volatile organic compounds in solid waste according to claim 1, wherein the internal standard in the step S3 is at least one of chlorobenzene-d 5, 1, 4-dichlorobenzene-d 4 and fluorobenzene.
8. The method for measuring volatile organic compounds in solid waste according to claim 3, wherein the fused silica capillary column is Agilent DB-VRX 30m x 0.25mm x 1.4 μm.
9. The method as claimed in claim 1, wherein the volatile organic compounds include dichloromethane, trimethylsilanol, 2-methylpentane, 3-methylpentane, n-hexane, 1-ethylcyclobutane, 1, 2-dichloroethane, 2-methylhexane, benzene, hexamethyldisiloxane, heptane, cyclohexane, dimethyldisulfide, sec-butyl acetate, toluene, butyl acetate, chlorobenzene, ethylbenzene, m-xylene, p-xylene, styrene, n-decane, 2,7, 7-tetramethyloctane, 2-ethylhexanol, tridecane, 2,3, 5-trimethylheptane, 2,6, 8-trimethyldecane, 2,3,5, 8-tetramethyldecane, 2, 6-dimethyldecane, 4-ethyloctane, toluene, 2-dimethyldecane, 2, 6-dimethyldecane, 2-ethylhexane, 2-dimethyldecane, 2-dimethyl, 2, 3-dimethyldecane, o-decylhydroxylamine, 2-methyldecane, acetone, ethanethiol, dimethylsulfide, 1-chloropropane, 2-chloropropane, 3-chloropropane, 2-butanone, 2-chlorobutane, methylcyclopentane, methanesulfonic acid, 3-methylhexane, 2,4, 6-trimethyloctane, 2, 4-dimethylhexane, 2,6, 11-trimethyldodecane, 2,7, 10-trimethyldodecane, 3-methyldecane, 4-methyloctane, diethyl methylthiophosphate, o-xylene, triethylthiophosphate, cis-4-cyclohexene-1, 2-dicarboxylic acid, and diethyl phosphite.
10. Use of the method for the determination of volatile organic compounds in solid waste according to any one of claims 1 to 9, characterized in that the method is used for the detection of volatile organic compounds in solid waste such as mining waste.
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