CN106841448A - A kind of detection method for polluting phenolic compound - Google Patents
A kind of detection method for polluting phenolic compound Download PDFInfo
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- CN106841448A CN106841448A CN201710085154.9A CN201710085154A CN106841448A CN 106841448 A CN106841448 A CN 106841448A CN 201710085154 A CN201710085154 A CN 201710085154A CN 106841448 A CN106841448 A CN 106841448A
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Abstract
The invention discloses a kind of detection method for polluting phenolic compound, detection method is as follows：（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, filtered using 0.22 μm of filter membrane after extracting, filtrate is obtained, it is standby；（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein SPE column volume is 2.6ml, seal the hole diameter of sieve (perforated) plate of extraction column for 0.7 1.6 μm, then addition eluent carries out wash-out extraction, extract is obtained, it is standby；（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then concentrated using Nitrogen evaporator, mixes and carry out chromatographic sample loading product after concentration and with acetonitrile sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatographic isolation, collect phenol mixture, it is standby；（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
Description
Technical field
The present invention relates to a kind of detection technique field, specifically a kind of detection method for polluting phenolic compound.
Background technology
In water body phenol pollution be mainly some industrial enterprises discharge phenol wastewater, such as coking, papermaking, plastics, dyestuff,
Many industry such as medicine, herbicide, agricultural chemicals, timber processing, when the concentration of phenol in water body reaches 0.1-0.2mg/L, this
Phenol will be contained in the fish body lived in water body, if people has eaten this fish, the phenol amount for taking in body exceedes the removing toxic substances energy of human body
During power, slow poisoning will occur, the symptoms such as headache, dizziness, vomiting, diarrhoea, neurological disorders, anaemia occur, with what is polluted
Water forms chlorophenol as drinking water in the presence of sterilization chlorine, and its taste is reinforced one to two orders of magnitude and produces stench,
Therefore by strict regulations, phenolic compound has the genotoxic potential of carcinogenic mutagenicity for the discharge of phenol.Both at home and abroad to quick, sensitive
The research for determining phenolic compound is very active.Gas chromatography is although sensitive, but needs derivative and extraction step and time-consuming,
Analyzed using HPLC- ultraviolet detections through a large amount of, but other coexist organic pollution and disturb larger, poor selectivity.
Phenols refers to the hydroxy derivatives of benzene and its condensed ring, and different phenolic compounds has different boiling points.According to it
Can be volatilized together with vapor and be divided into volatile phenol with non-volatile phenol.Volatile phenol typically refers to phenol of the boiling point below 230 DEG C
Class.The reliability and accuracy in analysis method are relied primarily on to the measure of pollutant.For the detection and analysis of phenolic compound,
Except traditional forint-Xi Mokate colorimetric methods (Folin-Ciocalteau colorimetry), many methods are based on purple
Outer AAS (UV-vis spectrophotometry), near-infrared spectrophotometry (Near-Infrared
Spectrometry), far infrared AAS (Far-Infrared Spectrometry), capillary electrophoresis
(Capillary Electrophoresi), gas chromatography (Gas Phase Chromatography), high performance liquid chromatography
Method (High Performance Liquid Chromatography) and gas chromatography-mass spectrography (Gas
Chromatography-Mass Spectrometry) etc. analysis method grow up.Because phenolic compound number of species is many
It is many, and trace and with high toxicity, therefore accurate delicately extraction from sample substrate reclaim and detection phenolic compound is
It is vital.Bromination volumetric method is used to determine concentration phenolic compound sample high, but operating procedure is numerous and diverse, and precision is not high；
4-APP AASs are the standard methods of volatile phenol detection, but analyze speed is slow, it is necessary to substantial amounts of organic extraction solvent, and
As bromination volumetric method, the content of total phenol can only be determined；Gas-chromatography and high performance liquid chromatography then have sensitivity higher
And accuracy, based on this, many micro- extractive techniques and Instrument crosslinking technology have also obtained extensive development.But these methods are both needed to
Want large-sized analytic instrument, it is impossible to online quick measure.Therefore, some quick analytical technologies, such as Flow Injection Analysis and continuous
Flow Analysis Technique is developed rapidly.Particularly biosensor technology, by improving constantly the sensitivity of detection and convenient
Property, the chlorophenols that have broad application prospects are the polluters being widely present in water environment, 2- chlorophenols, 2,3- dichloros
Phenol, the chlorophenols compound toxicity such as 2,4,6- trichlorophenols and pentachlorophenol is high, pollutes wide, it is difficult to degrade, therefore by Environmental Protection in America
Office (EPA) and China national Environmental Protection Administration list the blacklist of priority pollutants in.The monitoring method of chlorophenols is main
There is the method such as gas chromatography and liquid chromatogram ultraviolet detection.Gas chromatography determines chlorophenol and typically needs to derive, and process is complicated, and
Sensitivity is low, and the qualitative ability of liquid chromatogram ultraviolet detection is inaccurate.
Therefore the detection method of phenolic compound in the pollution that a kind of degree of accuracy is high, easy to operate, detectable limit is low is studied
It is necessary.
The content of the invention
It is an object of the invention to provide a kind of detection method for polluting phenolic compound, with solving above-mentioned background technology
The problem of proposition.
To achieve the above object, the present invention provides following technical scheme：
A kind of detection method for polluting phenolic compound, detection method is as follows：
（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, 0.22 μ is used after extracting
M filter membranes are filtered, and filtrate is obtained, standby；
（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein
SPE column volume is 2.6ml, seals the hole diameter of sieve (perforated) plate of extraction column for 0.7-1.6 μm, and then addition eluent is eluted
Extraction, is obtained extract, standby；
（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then carried out using Nitrogen evaporator dense
Contracting, mixes and carries out chromatographic sample loading product after concentration and with acetonitrile-sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatogram point
From, phenol mixture is collected, it is standby；
（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
As further scheme of the invention：Step（1）Temperature is 20-25 DEG C during middle extracting.
As further scheme of the invention：Step（2）Atomization gas use nitrogen, and atomization gas in middle ultrasonic atomizatio
Flow be 1.3m3/ h, and supersonic frequency is 1.2-1.4MHz.
As further scheme of the invention：Step（2）Middle eluent, in parts by weight, component be isopentane 5-12 parts,
Acetone 20-30 parts, petroleum ether 8-16 parts, pentamethylene 6-10 parts, carbon tetrachloride 2-6 parts, paraxylene 10-20 parts, butyl acetate
2-8 parts, methyl ethyl ketone 6-15 parts, acetonitrile 6-8 parts, isobutanol 6-12 parts.
As further scheme of the invention：Step（3）Nitrogen flow is 2m in middle Nitrogen evaporator3/h。
As further scheme of the invention：Step（3）In upper sample when by the flow velocity of chromatographic column be 0.8-1.2ml/
min。
As further scheme of the invention：Step（3）Middle chromatogram running parameter is as follows：Hexamethylene-dichloromethane is stream
Dynamic phase, flow velocity is 3.6mL/min, 22-26 DEG C of column temperature, input sample 20-30 μ l.
As further scheme of the invention：Step（4）Middle mass spectrum running parameter is as follows：Electron spray voltage is 4800V, from
Source temperature is 426 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：
Method has extraction efficiency high, simple to operate, the good, favorable reproducibility of selectivity, consumption reagent few and accuracy in the present invention
It is high.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of detection method for polluting phenolic compound, detection method is as follows：
（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, 0.22 μ is used after extracting
M filter membranes are filtered, and filtrate is obtained, standby；
（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein
SPE column volume is 2.6ml, seals the hole diameter of sieve (perforated) plate of extraction column for 0.7 μm, and then addition eluent carries out wash-out extraction,
Extract is obtained, it is standby；
（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then carried out using Nitrogen evaporator dense
Contracting, mixes and carries out chromatographic sample loading product after concentration and with acetonitrile-sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatogram point
From, phenol mixture is collected, it is standby；
（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
Preferably：Step（1）Temperature is 20 DEG C during middle extracting.
Preferably：Step（2）Atomization gas use nitrogen in middle ultrasonic atomizatio, and the flow of atomization gas is 1.3m3/ h,
And supersonic frequency is 1.2MHz.
Preferably：Step（2）Middle eluent, in parts by weight, component be 5 parts of isopentane, 20 parts of acetone, 8 parts of petroleum ether,
6 parts of pentamethylene, 2 parts of carbon tetrachloride, 10 parts of paraxylene, 2 parts of butyl acetate, 6 parts of methyl ethyl ketone, 6 parts of acetonitrile, isobutanol 6
Part.
Preferably：Step（3）Nitrogen flow is 2m in middle Nitrogen evaporator3/h。
Preferably：Step（3）In upper sample when by the flow velocity of chromatographic column be 0.8ml/min.
Preferably：Step（3）Middle chromatogram running parameter is as follows：Hexamethylene-dichloromethane is mobile phase, and flow velocity is 3.6mL/
Min, 22 DEG C of column temperature, the μ l of input sample 20.
Preferably：Step（4）Middle mass spectrum running parameter is as follows：Electron spray voltage is 4800V, and ion source temperature is 426 DEG C.
Embodiment 2
A kind of detection method for polluting phenolic compound, detection method is as follows：
（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, 0.22 μ is used after extracting
M filter membranes are filtered, and filtrate is obtained, standby；
（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein
SPE column volume is 2.6ml, seals the hole diameter of sieve (perforated) plate of extraction column for 0.9 μm, and then addition eluent carries out wash-out extraction,
Extract is obtained, it is standby；
（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then carried out using Nitrogen evaporator dense
Contracting, mixes and carries out chromatographic sample loading product after concentration and with acetonitrile-sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatogram point
From, phenol mixture is collected, it is standby；
（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
Preferably：Step（1）Temperature is 22 DEG C during middle extracting.
Preferably：Step（2）Atomization gas use nitrogen in middle ultrasonic atomizatio, and the flow of atomization gas is 1.3m3/ h,
And supersonic frequency is 1.3MHz.
Preferably：Step（2）Middle eluent, in parts by weight, component is 6 parts of isopentane, 22 parts of acetone, petroleum ether 11
Part, 8 parts of pentamethylene, 3 parts of carbon tetrachloride, 15 parts of paraxylene, 3 parts of butyl acetate, 8 parts of methyl ethyl ketone, 6 parts of acetonitrile, isobutyl
9 parts of alcohol.
Preferably：Step（3）Nitrogen flow is 2m in middle Nitrogen evaporator3/h。
Preferably：Step（3）In upper sample when by the flow velocity of chromatographic column be 0.9ml/min.
Preferably：Step（3）Middle chromatogram running parameter is as follows：Hexamethylene-dichloromethane is mobile phase, and flow velocity is 3.6mL/
Min, 23 DEG C of column temperature, the μ l of input sample 22.
Preferably：Step（4）Middle mass spectrum running parameter is as follows：Electron spray voltage is 4800V, and ion source temperature is 426 DEG C.
Embodiment 3
A kind of detection method for polluting phenolic compound, detection method is as follows：
（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, 0.22 μ is used after extracting
M filter membranes are filtered, and filtrate is obtained, standby；
（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein
SPE column volume is 2.6ml, seals the hole diameter of sieve (perforated) plate of extraction column for 1.2 μm, and then addition eluent carries out wash-out extraction,
Extract is obtained, it is standby；
（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then carried out using Nitrogen evaporator dense
Contracting, mixes and carries out chromatographic sample loading product after concentration and with acetonitrile-sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatogram point
From, phenol mixture is collected, it is standby；
（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
Preferably：Step（1）Temperature is 23 DEG C during middle extracting.
Preferably：Step（2）Atomization gas use nitrogen in middle ultrasonic atomizatio, and the flow of atomization gas is 1.3m3/ h,
And supersonic frequency is 1.3MHz.
Preferably：Step（2）Middle eluent, in parts by weight, component is 9 parts of isopentane, 25 parts of acetone, petroleum ether 14
Part, 8 parts of pentamethylene, 4 parts of carbon tetrachloride, 15 parts of paraxylene, 5 parts of butyl acetate, 10 parts of methyl ethyl ketone, 7 parts of acetonitrile, isobutyl
9 parts of alcohol.
Preferably：Step（3）Nitrogen flow is 2m in middle Nitrogen evaporator3/h。
Preferably：Step（3）In upper sample when by the flow velocity of chromatographic column be 1.0ml/min.
Preferably：Step（3）Middle chromatogram running parameter is as follows：Hexamethylene-dichloromethane is mobile phase, and flow velocity is 3.6mL/
Min, 24 DEG C of column temperature, the μ l of input sample 25.
Preferably：Step（4）Middle mass spectrum running parameter is as follows：Electron spray voltage is 4800V, and ion source temperature is 426 DEG C.
Embodiment 4
A kind of detection method for polluting phenolic compound, detection method is as follows：
（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, 0.22 μ is used after extracting
M filter membranes are filtered, and filtrate is obtained, standby；
（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein
SPE column volume is 2.6ml, seals the hole diameter of sieve (perforated) plate of extraction column for 1.3 μm, and then addition eluent carries out wash-out extraction,
Extract is obtained, it is standby；
（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then carried out using Nitrogen evaporator dense
Contracting, mixes and carries out chromatographic sample loading product after concentration and with acetonitrile-sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatogram point
From, phenol mixture is collected, it is standby；
（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
Preferably：Step（1）Temperature is 24 DEG C during middle extracting.
Preferably：Step（2）Atomization gas use nitrogen in middle ultrasonic atomizatio, and the flow of atomization gas is 1.3m3/ h,
And supersonic frequency is 1.4MHz.
Preferably：Step（2）Middle eluent, in parts by weight, component is 10 parts of isopentane, 27 parts of acetone, petroleum ether 14
Part, 9 parts of pentamethylene, 5 parts of carbon tetrachloride, 18 parts of paraxylene, 7 parts of butyl acetate, 13 parts of methyl ethyl ketone, 7 parts of acetonitrile, isobutyl
11 parts of alcohol.
Preferably：Step（3）Nitrogen flow is 2m in middle Nitrogen evaporator3/h。
Preferably：Step（3）In upper sample when by the flow velocity of chromatographic column be 1.1ml/min.
Preferably：Step（3）Middle chromatogram running parameter is as follows：Hexamethylene-dichloromethane is mobile phase, and flow velocity is 3.6mL/
Min, 25 DEG C of column temperature, the μ l of input sample 28.
Preferably：Step（4）Middle mass spectrum running parameter is as follows：Electron spray voltage is 4800V, and ion source temperature is 426 DEG C.
Embodiment 5
A kind of detection method for polluting phenolic compound, detection method is as follows：
（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, 0.22 μ is used after extracting
M filter membranes are filtered, and filtrate is obtained, standby；
（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein
SPE column volume is 2.6ml, seals the hole diameter of sieve (perforated) plate of extraction column for 1.6 μm, and then addition eluent carries out wash-out extraction,
Extract is obtained, it is standby；
（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then carried out using Nitrogen evaporator dense
Contracting, mixes and carries out chromatographic sample loading product after concentration and with acetonitrile-sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatogram point
From, phenol mixture is collected, it is standby；
（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
Preferably：Step（1）Temperature is 25 DEG C during middle extracting.
Preferably：Step（2）Atomization gas use nitrogen in middle ultrasonic atomizatio, and the flow of atomization gas is 1.3m3/ h,
And supersonic frequency is 1.4MHz.
Preferably：Step（2）Middle eluent, in parts by weight, component is 12 parts of isopentane, 30 parts of acetone, petroleum ether 16
It is part, 10 parts of pentamethylene, 6 parts of carbon tetrachloride, 20 parts of paraxylene, 8 parts of butyl acetate, 15 parts of methyl ethyl ketone, 8 parts of acetonitrile, different
12 parts of butanol.
Preferably：Step（3）Nitrogen flow is 2m in middle Nitrogen evaporator3/h。
Preferably：Step（3）In upper sample when by the flow velocity of chromatographic column be 1.2ml/min.
Preferably：Step（3）Middle chromatogram running parameter is as follows：Hexamethylene-dichloromethane is mobile phase, and flow velocity is 3.6mL/
Min, 26 DEG C of column temperature, the μ l of input sample 30.
Preferably：Step（4）Middle mass spectrum running parameter is as follows：Electron spray voltage is 4800V, and ion source temperature is 426 DEG C.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires to be limited rather than described above, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each implementation method is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Specification an as entirety, the technical scheme in each embodiment can also be formed into those skilled in the art through appropriately combined
May be appreciated other embodiment.
Claims (8)
1. it is a kind of pollute phenolic compound detection method, it is characterised in that detection method is as follows：
（1）Sample pre-treatments：Pollution phenolic compound is enriched with, and is stripped using ethanol, 0.22 μ is used after extracting
M filter membranes are filtered, and filtrate is obtained, standby；
（2）SPE：Filtrate is carried out into ultrasonic atomizatio at room temperature, is transferred in solid-phase extraction column after ultrasonic atomizatio, wherein
SPE column volume is 2.6ml, seals the hole diameter of sieve (perforated) plate of extraction column for 0.7-1.6 μm, and then addition eluent is eluted
Extraction, is obtained extract, standby；
（3）Chromatographic isolation：Extract is used into methyl alcohol drip washing, drip washing temperature is no more than 10 DEG C, is then carried out using Nitrogen evaporator dense
Contracting, mixes and carries out chromatographic sample loading product after concentration and with acetonitrile-sodium dihydrogen phosphate, setting chromatogram running parameter carries out chromatogram point
From, phenol mixture is collected, it is standby；
（4）Mass Spectrometric Identification：Phenol mixture is injected into mass spectrograph, setting mass spectrum running parameter carries out Mass Spectrometric Identification.
2. it is according to claim 1 pollution phenolic compound detection method, it is characterised in that step（1）During middle extracting
Temperature is 20-25 DEG C.
3. it is according to claim 1 pollution phenolic compound detection method, it is characterised in that step（2）Middle ultrasonic mist
Atomization gas use nitrogen in change, and the flow of atomization gas is 1.3m3/ h, and supersonic frequency is 1.2-1.4MHz.
4. it is according to claim 1 pollution phenolic compound detection method, it is characterised in that step（2）Middle eluent,
In parts by weight, component is isopentane 5-12 parts, acetone 20-30 parts, petroleum ether 8-16 parts, pentamethylene 6-10 parts, carbon tetrachloride
2-6 parts, paraxylene 10-20 parts, butyl acetate 2-8 parts, methyl ethyl ketone 6-15 parts, acetonitrile 6-8 parts, isobutanol 6-12 parts.
5. it is according to claim 1 pollution phenolic compound detection method, it is characterised in that step（3）Middle Nitrogen evaporator
Middle nitrogen flow is 2m3/h。
6. it is according to claim 1 pollution phenolic compound detection method, it is characterised in that step（3）In upper sample
When by the flow velocity of chromatographic column be 0.8-1.2ml/min.
7. it is according to claim 1 pollution phenolic compound detection method, it is characterised in that step（3）Middle chromatogram work
Make parameter as follows：Hexamethylene-dichloromethane is mobile phase, and flow velocity is 3.6mL/min, 22-26 DEG C of column temperature, input sample 20-30 μ l.
8. it is according to claim 1 pollution phenolic compound detection method, it is characterised in that step（4）Middle mass spectrum work
Make parameter as follows：Electron spray voltage is 4800V, and ion source temperature is 426 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109839449A (en) * | 2017-11-28 | 2019-06-04 | 中国石油天然气股份有限公司 | The method of phenolic compound in Solid phase extraction separation diesel oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109839449A (en) * | 2017-11-28 | 2019-06-04 | 中国石油天然气股份有限公司 | The method of phenolic compound in Solid phase extraction separation diesel oil |
| CN109839449B (en) * | 2017-11-28 | 2021-11-30 | 中国石油天然气股份有限公司 | Method for separating phenolic compounds in diesel oil by solid phase extraction |
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