CN111896667A - Method for detecting 16 polycyclic aromatic hydrocarbons in heat insulation coating - Google Patents
Method for detecting 16 polycyclic aromatic hydrocarbons in heat insulation coating Download PDFInfo
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- CN111896667A CN111896667A CN202010859798.0A CN202010859798A CN111896667A CN 111896667 A CN111896667 A CN 111896667A CN 202010859798 A CN202010859798 A CN 202010859798A CN 111896667 A CN111896667 A CN 111896667A
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- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 title claims abstract description 59
- 238000000576 coating method Methods 0.000 title claims abstract description 43
- 239000011248 coating agent Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000009413 insulation Methods 0.000 title claims abstract description 21
- 238000001514 detection method Methods 0.000 claims abstract description 40
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 9
- SPWVRYZQLGQKGK-UHFFFAOYSA-N dichloromethane;hexane Chemical compound ClCCl.CCCCCC SPWVRYZQLGQKGK-UHFFFAOYSA-N 0.000 claims abstract description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000003463 adsorbent Substances 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
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- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
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- DXBHBZVCASKNBY-UHFFFAOYSA-N 1,2-Benz(a)anthracene Chemical compound C1=CC=C2C3=CC4=CC=CC=C4C=C3C=CC2=C1 DXBHBZVCASKNBY-UHFFFAOYSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Chemical compound C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- KHNYNFUTFKJLDD-UHFFFAOYSA-N BCR-49 Natural products C1=CC(C=2C3=CC=CC=C3C=CC=22)=C3C2=CC=CC3=C1 KHNYNFUTFKJLDD-UHFFFAOYSA-N 0.000 description 2
- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 description 2
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- HAXBIWFMXWRORI-UHFFFAOYSA-N Benzo[k]fluoranthene Chemical compound C1=CC(C2=CC3=CC=CC=C3C=C22)=C3C2=CC=CC3=C1 HAXBIWFMXWRORI-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- WDECIBYCCFPHNR-UHFFFAOYSA-N chrysene Chemical compound C1=CC=CC2=CC=C3C4=CC=CC=C4C=CC3=C21 WDECIBYCCFPHNR-UHFFFAOYSA-N 0.000 description 2
- LHRCREOYAASXPZ-UHFFFAOYSA-N dibenz[a,h]anthracene Chemical compound C1=CC=C2C(C=C3C=CC=4C(C3=C3)=CC=CC=4)=C3C=CC2=C1 LHRCREOYAASXPZ-UHFFFAOYSA-N 0.000 description 2
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- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
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- TXVHTIQJNYSSKO-UHFFFAOYSA-N BeP Natural products C1=CC=C2C3=CC=CC=C3C3=CC=CC4=CC=C1C2=C34 TXVHTIQJNYSSKO-UHFFFAOYSA-N 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 125000004054 acenaphthylenyl group Chemical group C1(=CC2=CC=CC3=CC=CC1=C23)* 0.000 description 1
- HXGDTGSAIMULJN-UHFFFAOYSA-N acetnaphthylene Natural products C1=CC(C=C2)=C3C2=CC=CC3=C1 HXGDTGSAIMULJN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
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- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YWSOTAXHDWRACQ-UHFFFAOYSA-N benzene;1h-indene Chemical compound C1=CC=CC=C1.C1=CC=C2CC=CC2=C1 YWSOTAXHDWRACQ-UHFFFAOYSA-N 0.000 description 1
- FTOVXSOBNPWTSH-UHFFFAOYSA-N benzo[b]fluoranthene Chemical compound C12=CC=CC=C1C1=CC3=CC=CC=C3C3=C1C2=CC=C3 FTOVXSOBNPWTSH-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
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- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
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- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- RMBPEFMHABBEKP-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2C3=C[CH]C=CC3=CC2=C1 RMBPEFMHABBEKP-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
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- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
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- NIHNNTQXNPWCJQ-UHFFFAOYSA-N o-biphenylenemethane Natural products C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/143—Preparation by elimination of some components selective absorption
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
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Abstract
The invention discloses a method for detecting 16 polycyclic aromatic hydrocarbons in a heat insulation coating, which comprises the following specific steps: adding a dichloromethane-n-hexane solution with the volume ratio of 1 (1-1.5) to ultrasonically extract polycyclic aromatic hydrocarbon in the heat insulation coating at the temperature of 35-40 ℃; then the extract is purified by adding anhydrous magnesium sulfate, C18, PSA and GCB by QuEChERS method; and finally, making a standard curve of the polycyclic aromatic hydrocarbon, detecting the purified sample by a high performance liquid chromatography, and calculating by combining the standard curve to obtain the concentration of the polycyclic aromatic hydrocarbon in the heat insulation coating. The method has the advantages of high recovery rate of polycyclic aromatic hydrocarbon in the heat-insulating coating, good purification effect, reduction of the influence of impurities on the detection result, improvement of the detection precision of the sample, higher final sample labeling recovery rate and precision, more stable detection result, short detection time and low cost.
Description
Technical Field
The invention belongs to the technical field of detection of organic pollutants of building materials, and particularly relates to a method for detecting 16 polycyclic aromatic hydrocarbons in a heat insulation coating.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) are aromatic compounds containing 2 or more benzene rings. The polycyclic aromatic hydrocarbon is mostly colorless crystals, and a small part of the polycyclic aromatic hydrocarbon is dark,high melting point and boiling point, low vapor pressure, most of which are insoluble in water, slightly soluble in organic solvent, and easily soluble in benzene aromatic solvent, and has the characteristics of volatility or semi-volatility, high hydrophobicity and low degradability[23]. Currently, over 200 PAHs are known, and the most widely studied PAHs are 16 PAHs pollutants with priority control, EPA16 for short, proposed by the U.S. environmental protection agency in 1976 as shown in the following Table 1:
TABLE 1EPA16 polycyclic aromatic hydrocarbons
In nature, forest fire and volcanic eruption are the most main modes for generating polycyclic aromatic hydrocarbon, but in modern society, due to the development of modern industry, chemical and biological fuels are used in large quantities in the industrial production process, and a large amount of polycyclic aromatic hydrocarbon byproducts are generated. Research shows that polycyclic aromatic hydrocarbon has carcinogenic, teratogenic and mutagenic 'triple-causing' effects, and can induce canceration of lung, liver and other parts through the digestive system of human body after entering human body.
The paint is an important decoration product based on petrochemical industry as raw materials, and is widely applied to daily life. However, organic solvents are inevitably added in the production and processing processes of the coating, and polycyclic aromatic hydrocarbons in the organic pollutants become a non-negligible part of the coating and can cause irreversible damage and threat to the environment and human bodies. Therefore, the detection of the polycyclic aromatic hydrocarbon substances in the coating has very important significance for guaranteeing the health of consumers and standardizing the coating market field.
In recent years, though research on polycyclic aromatic hydrocarbons by various research units is more intensive, the research is only in the fields of environment, rubber and plastics and food, but the research is rarely reported in the aspect of coatings. The heat insulation coating mainly comprises organic emulsion, inorganic pigment and filler, water, various coating additives and the like, and is characterized in that the raw materials are various, the components are very complex, and the content of polycyclic aromatic hydrocarbon is low, so that the extraction and purification difficulty in the detection process is high, and the detection precision is difficult to grasp. In the detection of polycyclic aromatic hydrocarbons in the coating specified in GB/T36488-2018 'determination of polycyclic aromatic hydrocarbons in coating' published in 2018, n-hexane is used as an extracting agent, and after centrifugal extraction, purification treatment is not carried out, and the detection is directly carried out by adopting a GC-MS method.
Disclosure of Invention
The invention aims to provide a method for detecting 16 polycyclic aromatic hydrocarbons in a heat-insulating and heat-preserving coating, which has the advantages of high recovery rate of the polycyclic aromatic hydrocarbons in the heat-insulating and heat-preserving coating, good purification effect, reduction of the influence of impurities on a detection result, improvement of the detection precision of a sample, higher final sample standard addition recovery rate and precision, more stable detection result, short detection time and low cost.
In order to solve the technical problems, the invention adopts the following technical scheme:
the method for detecting 16 polycyclic aromatic hydrocarbons in the heat insulation coating comprises the following steps:
(1) extraction of polycyclic aromatic hydrocarbons: adding a dichloromethane-n-hexane mixed solvent with a volume ratio of 1 (1-1.5) into a heat insulation coating, shaking by hand for 1-2min, and then performing ultrasonic extraction at 35-40 ℃ for 30-40min to obtain a supernatant, wherein the mass volume ratio of the heat insulation coating to the dichloromethane-n-hexane mixed solvent is 1 (5-10);
(2) QuEChERS method purification: taking the supernatant obtained in the step (1), respectively adding solid phase adsorbent anhydrous magnesium sulfate, C18, PSA and GCB, then centrifuging, absorbing the supernatant into a sample injection bottle after centrifuging, and filtering with a 0.22um filter membrane;
(3) detecting by a high performance liquid chromatography: and (3) making standard curves of 16 kinds of polycyclic aromatic hydrocarbons, detecting the sample obtained in the step (2) by a high performance liquid chromatography method, and calculating by combining the standard curves to obtain the concentration of the polycyclic aromatic hydrocarbons in the heat insulation coating.
According to the scheme, in the step (2), the use amounts of the anhydrous magnesium sulfate, the C18, the PSA and the GCB adsorbent account for 15-20%, 10-15%, 5-10% and 5-10% of the clear liquid to be purified respectively by mass percent.
According to the scheme, in the step (2), the centrifugation parameter is 3000-5000r/min, and the time is 5-8 min.
According to the scheme, in the step (2), the 0.22um filter membrane is a 0.22um organic phase filter membrane.
According to the scheme, in the step (3), the detection conditions of the high performance liquid chromatography method are as follows: c18 column, 50mm X2.1 mm inner diameter; the granularity is 1.7 mm; column temperature, 30 ℃; sample size, 20 ul; the mobile phase is acetonitrile and water in a volume ratio of 60: 40; the flow rate is 1.0 ml/min; the wavelength is 230 nm.
According to the scheme, in the step (3), the standard curves of the 16 polycyclic aromatic hydrocarbons are prepared by the following steps: accurately weighing 0.0500g of polycyclic aromatic hydrocarbon standard, metering the volume to 500ml by using chromatographic methanol, preparing 100mg/L standard mother liquor, then respectively preparing 5, 1, 0.5 and 0.2mg/L standard solutions, repeatedly injecting the sample for three times when detecting the high performance liquid, quantitatively calculating by adopting an external standard method, and drawing a standard curve according to the relation between the injection concentration and the peak area.
The method adopts the mixed solvent of normal hexane and dichloromethane to extract 16 polycyclic aromatic hydrocarbons in the heat-insulating coating at a temperature slightly higher than room temperature (35-40 ℃), has better extraction effect, can effectively extract polycyclic aromatic hydrocarbons with larger molecular weight and larger polarity, such as benzo (k) fluoranthene, dibenzo (a, h) anthracene, indene benzene (1,2,3-cd) pyrene and the like, can reduce the dissolution of impurities such as resin with higher content in the coating, and the like, and improves the recovery rate of the polycyclic aromatic hydrocarbons in the heat-insulating coating. And the impurities in the sample can be quickly, efficiently and simply adsorbed by adopting the QuEChERS method for purification, the influence of the impurities on the detection result is reduced, and the detection precision of the sample is improved, wherein anhydrous magnesium sulfate in the adsorbent is used for removing water in the heat-insulating coating, PSA is mainly used for adsorbing some impurities in the heat-insulating coating, such as carbohydrates, fatty acids, organic acids, phenols and the like, C18 is used for removing solid interferents, such as fats, esters, calcium carbonate, hollow glass beads and the like in heat-insulating filling materials, and GCB is mainly used for removing sterols and non-polar interferents in the matrix. And finally, the detection is carried out by using a high performance liquid chromatography, so that the detection cost is greatly reduced, the final sample standard adding recovery rate and precision are high, and the detection result is stable.
The invention has the beneficial effects that:
the method adopts a dichloromethane-n-hexane mixed solvent to extract the polycyclic aromatic hydrocarbon in the heat-insulating coating at a temperature slightly higher than room temperature (35-40 ℃), can extract the target polycyclic aromatic hydrocarbon as much as possible and extract impurities as little as possible, and improves the recovery rate of the polycyclic aromatic hydrocarbon in the heat-insulating coating; then, the QuEChERS method is adopted for purification, and the anhydrous magnesium sulfate, PSA, C18 and GCB adsorbents can quickly, efficiently and simply adsorb water and impurities in the sample, so that the influence of the impurities on the detection result is reduced, and the detection precision of the sample is improved; and finally, detecting by using a high performance liquid chromatography, so that the detection cost is greatly reduced, the final sample standard adding recovery rate and precision are high, the detection result is stable, and the standard adding recovery rate of the method is between 81.2 and 104.6 percent and the relative standard deviation is between 1.4 and 9.7 percent by calculation.
Detailed Description
In order to make the purpose, technical solution and advantages of the present invention more clear, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preparation of standard curves for 16 polycyclic aromatic hydrocarbons: respectively and accurately weighing 0.0500g of polycyclic aromatic hydrocarbon (naphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene, chrysene, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, dibenzo (a, h) anthracene, benzo (g, h, i) perylene and indene (1,2,3-cd) pyrene) standard substance (the purity is more than or equal to 99.9%), using chromatographic methanol to fix the volume to 500ml, preparing 100mg/L standard mother liquor, then respectively preparing 5, 1, 0.5 and 0.2mg/L standard solutions, after high performance liquid detection (the concentration of each group is repeatedly injected for three times), adopting an external standard method to quantitatively calculate, and drawing a standard curve according to the relation between the injection concentration and peak area.
Determination of recovery: adding 16 polycyclic aromatic hydrocarbon standard solutions into a heat preservation coating sample, respectively adding the 16 polycyclic aromatic hydrocarbon standard solutions into the heat preservation coating sample to be 0.050, 0.100 and 0.500mg/kg, then taking a sample without the added standard solution in the same amount as a control group, carrying out extraction purification and detection according to an established method, wherein the sample without the added standard solution is used as a matrix blank for calculating the content and recovery rate of the polycyclic aromatic hydrocarbon in the sample, repeating the experiment of each group for three times, and taking an average value.
The recovery and precision of 16 polycyclic aromatic hydrocarbons are shown in table 2, and the detection limit and the quantification limit are shown in table 3:
TABLE 2 recovery and precision of 16 polycyclic aromatic hydrocarbons in the thermal insulation coating
TABLE 3 detection limit and quantitative limit of polycyclic aromatic hydrocarbons in 16 of thermal insulation coating
Example 1
The method for detecting the polycyclic aromatic hydrocarbon in the heat insulation coating comprises the following steps:
(1) extraction of polycyclic aromatic hydrocarbons: accurately weighing 5.00g of the coating in a 50ml centrifuge tube with a plug by using an electronic balance, adding 30ml of dichloromethane-n-hexane (1:1) solution into the centrifuge tube, covering the cover of the centrifuge tube, shaking by hand for 1min, and performing ultrasonic extraction at 35 ℃ for 40min to obtain a supernatant.
(2) QuEChERS method purification: and (2) sucking 3ml of the supernatant obtained in the step (1) into a centrifuge tube, adding 450mg of anhydrous magnesium sulfate, 300mgC18, 150mg of PSA and 150mg of GCB solid phase adsorbent respectively, centrifuging, sucking the supernatant into a 2ml sample bottle, filtering with a 0.22um organic phase filter membrane, and detecting.
(3) High performance liquid detection: detecting by adopting a high performance liquid chromatography, wherein the detection conditions are as follows: a C18 column, 50mm by 2.1mm (internal diameter); the granularity is 1.7 mm; column temperature, 30 ℃; sample size, 20 ul; the mobile phase is acetonitrile and water (60: 40); the flow rate is 1.0 ml/min; the wavelength is 230 nm. The results are shown in Table 4.
Table 4 content of polycyclic aromatic hydrocarbon in 16 of thermal insulation coating in example 1
Note: no detection of N.D., the same as
Example 2
The method for detecting the polycyclic aromatic hydrocarbon in the heat insulation coating comprises the following steps:
(1) extraction of polycyclic aromatic hydrocarbons: accurately weighing 10.00g of the coating in a 50ml centrifuge tube with a plug by using an electronic balance, adding 40ml of dichloromethane-n-hexane (1:1) solution into the centrifuge tube, covering the cover of the centrifuge tube, shaking by hand for 1min, and performing ultrasonic extraction at 35 ℃ for 40min to obtain a supernatant.
(2) QuEChERS method purification: and (2) sucking 3ml of the supernatant obtained in the step (1) into a centrifuge tube, adding 600mg of anhydrous magnesium sulfate, 450mgC18, 300mg of PSA and 300mg of GCB solid phase adsorbent respectively, centrifuging, sucking the supernatant into a 2ml sample bottle, filtering with a 0.22um organic phase filter membrane, and detecting.
(3) High performance liquid detection: detecting by adopting a high performance liquid chromatography, wherein the detection conditions are as follows: a C18 column, 50mm by 2.1mm (internal diameter); the granularity is 1.7 mm; column temperature, 30 ℃; sample size, 20 ul; the mobile phase is acetonitrile and water (60: 40); the flow rate is 1.0 ml/min; the wavelength is 230 nm. The results are shown in Table 5.
TABLE 5 content of polycyclic aromatic hydrocarbons in 16 of the thermal insulation coating in example 2
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A detection method for 16 polycyclic aromatic hydrocarbons in a heat insulation coating is characterized by comprising the following steps:
(1) extraction of polycyclic aromatic hydrocarbons: adding a dichloromethane-n-hexane mixed solvent with a volume ratio of 1 (1-1.5) into a heat insulation coating, shaking by hand for 1-2min, and then performing ultrasonic extraction at 35-40 ℃ for 30-40min to obtain a supernatant, wherein the mass volume ratio of the heat insulation coating to the dichloromethane-n-hexane mixed solvent is 1 (5-10);
(2) QuEChERS method purification: taking the supernatant obtained in the step (1), respectively adding solid phase adsorbent anhydrous magnesium sulfate, C18, PSA and GCB, then centrifuging, absorbing the supernatant into a sample injection bottle after centrifuging, and filtering with a 0.22um filter membrane;
(3) detecting by a high performance liquid chromatography: and (3) making standard curves of 16 kinds of polycyclic aromatic hydrocarbons, detecting the sample obtained in the step (2) by a high performance liquid chromatography method, and calculating by combining the standard curves to obtain the concentration of the polycyclic aromatic hydrocarbons in the heat insulation coating.
2. The detection method according to claim 1, wherein in the step (2), the use amounts of the anhydrous magnesium sulfate, the C18, the PSA and the GCB adsorbents account for 15-20%, 10-15%, 5-10% and 5-10% of the clear liquid to be purified respectively by mass percent.
3. The detection method as claimed in claim 1, wherein in the step (2), the centrifugation parameter is 3000-5000r/min, and the time is 5-8 min.
4. The detection method according to claim 1, wherein in the step (2), the 0.22um filter is a 0.22um organic phase filter.
5. The detection method according to claim 1, wherein in the step (3), the detection conditions of the high performance liquid chromatography are as follows: c18 column, 50mm X2.1 mm inner diameter; the granularity is 1.7 mm; column temperature, 30 ℃; sample size, 20 ul; the mobile phase is acetonitrile and water in a volume ratio of 60: 40; the flow rate is 1.0 ml/min; the wavelength is 230 nm.
6. The detection method according to claim 1, wherein in the step (3), the standard curve preparation steps for 16 polycyclic aromatic hydrocarbons are as follows: accurately weighing 0.0500g of polycyclic aromatic hydrocarbon standard, metering the volume to 500ml by using chromatographic methanol, preparing 100mg/L standard mother liquor, then respectively preparing 5, 1, 0.5 and 0.2mg/L standard solutions, repeatedly injecting the sample for three times when detecting the high performance liquid, quantitatively calculating by adopting an external standard method, and drawing a standard curve according to the relation between the injection concentration and the peak area.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104181254A (en) * | 2014-09-03 | 2014-12-03 | 云南中烟工业有限责任公司 | Method for determining polycyclic aromatic hydrocarbon in hot melt adhesive by separation |
| CN105466737A (en) * | 2015-12-29 | 2016-04-06 | 河海大学 | Passive sampler for gaseous polycyclic aromatic hydrocarbon in root box experiment and sample determining method thereof |
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|---|---|---|---|---|
| CN104181254A (en) * | 2014-09-03 | 2014-12-03 | 云南中烟工业有限责任公司 | Method for determining polycyclic aromatic hydrocarbon in hot melt adhesive by separation |
| CN105466737A (en) * | 2015-12-29 | 2016-04-06 | 河海大学 | Passive sampler for gaseous polycyclic aromatic hydrocarbon in root box experiment and sample determining method thereof |
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| Title |
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| 万译文等: "QuEChERS/高效液相色谱法同时测定水产品中16种多环芳烃", 《湖南师范大学自然科学学报》 * |
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