CN106645448A - Separation detection method of phenol compounds in textiles - Google Patents
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- CN106645448A CN106645448A CN201610861339.XA CN201610861339A CN106645448A CN 106645448 A CN106645448 A CN 106645448A CN 201610861339 A CN201610861339 A CN 201610861339A CN 106645448 A CN106645448 A CN 106645448A
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Abstract
The invention relates to a separation detection method of phenol compounds in textiles. The separation detection method includes following steps: taking and adding a to-be-detected textile sample into an extraction kettle, adding a derivatization reagent or adding a derivatization reagent and a cosolvent, performing supercritical carbon dioxide extraction at temperature of 40-90 DEG C and pressure of 15-45MPa on the to-be-detected textile sample, and collecting to obtain an extract; using an organic solvent to dissolve the extract to obtain an extract solution, adding a potassium carbonate solution, shaking, and using a drying agent to dry an organic phase to obtain a to-be-detected sample solution; detecting the phenol compounds in the to-be-detected sample solution. The separation detection method is low in solvent consumption during pretreatment and environment-friendly, has the advantages of quickness, high repeatability and simple operation, can detect various chlorine-containing phenol and o-phenylphenol at the same time and is high in recycling rate of the phenol compounds.
Description
Technical field
The present invention relates to textile and analysis detection field, phenol compound in more particularly to a kind of textile
Method for separating and detecting.
Background technology
The phenol compound that may contain in textile mainly has containing chlorophenols compound (pentachlorophenol (PCP), tetrachloro
Phenol (TeCP), trichlorophenol, 2,4,6,-T (TrCP), chlorophenesic acid (DCP), monochloro phenol (MCP)) and o-phenyl phenol (OPP) etc., this
A little compounds are commonly used for antibacterial and preservative.These compounds are respectively provided with certain bio-toxicity effect, can be to environment and people
Body health produces impact, therefore, its residue problem in textiles and leathers receives much concern.As relevant toxicity and toxicity grind
That what is studied carefully deepens continuously, and the residue limits of relevant law, regulation and standard to which in textile have strict restriction.Germany is right
The limitation requirement of TeCP and PCP：Product with direct skin contact is 0.05mg/kg, with the product of direct skin contact is not
5mg/kg；Limitation requirement of the France to PCP：Product with direct skin contact is 0.5mg/kg, not with direct skin contact
Product is 5mg/kg；Holland and Austria are 5mg/kg to the limitation of PCP；Switzerland is 10mg/kg to the limitation of PCP and TeCP；
To totally 19 kinds of the limitation requirement of all chlorinated phenols from a chlorine to pentachloro- in Oeko-Tex 100 (2016)：TeCP and PCP are in I
It is 0.05mg/kg in class product, is 0.5mg/kg in II class, III class and IV class product, TrCP is 0.2mg/ in I class products
Kg, in II class, III class and IV class product for 2.0mg/kg, DCP and MCP in I class products be 0.5mg/kg, II class, III class and
It is 3.0mg/kg in IV class product, OPP is 50.0mg/kg in I class products, is in II class, III class and IV class product
100.0mg/kg.China standard GB/T 18885-2009 has also carried out strict restriction to PCP, TeCP and OPP.
At present, measure is through surname extraction, supersound extraction containing chlorophenol, the main method of o-phenyl phenol or adds both at home and abroad
After quick-dissolving agent is extracted, perform the derivatization, then using gas chromatogram-electron capture detector (ECD) (GC-ECD) or gas chromatogram-quality
Detector (GC-MS) is selected to determine.These technologies presence can not detect the various defects containing chlorophenol Yu o-phenyl phenol simultaneously, and
With the defect such as time-consuming, organic solvent usage amount is big.
The content of the invention
Based on this, the invention provides in a kind of textile phenol compound method for separating and detecting, the detection method
Have the advantages that quick, solvent load is few, environmental protection.
Concrete technical scheme is as follows：
In a kind of textile, the method for separating and detecting of phenol compound, comprises the following steps：
Take textile samples to be measured to be added in extraction kettle, addition derivatization reagent or addition derivatization reagent are molten with common
Textile samples to be measured are carried out supercritical carbon dioxide extraction by agent, and collection obtains extract；The supercritical carbon dioxide extraction
The temperature for taking is 40～90 DEG C, and pressure is 15～45MPa；
Extract organic solvent is dissolved, extract solution is obtained, solution of potassium carbonate, shaking, organic faciess drying is added
Agent is dried, and obtains testing sample solution；
Phenol compound in detection testing sample solution.
Wherein in some embodiments, the process of the supercritical carbon dioxide extraction be 25～40min of dynamic extraction or
Person elder generation 5～30min of static extracting, then 10～20min of dynamic extraction；During static extracting, the supercritical carbon dioxide with it is described
The proportioning of textile samples to be measured is 2-4mL：1g；During dynamic extraction, the flow velocity of the supercritical carbon dioxide is 1～10mL/
min。
Wherein in some embodiments, the process of the supercritical carbon dioxide extraction is 8～15min of first static extracting,
10～20min of dynamic extraction again；During dynamic extraction, the flow velocity of the supercritical carbon dioxide is 1.5～2.5mL/min.
Wherein in some embodiments, the temperature of the supercritical carbon dioxide extraction is 45～55 DEG C, pressure is 30～
40MPa。
Wherein in some embodiments, the derivatization reagent is acetic anhydride, the derivatization reagent and the spinning to be measured
The proportioning of fabric sample is 10～50 μ L：1g.
Wherein in some embodiments, the derivatization reagent is 45～50 μ with the proportioning of the textile samples to be measured
L：1g.
Wherein in some embodiments, the cosolvent in benzene, dichloromethane, methanol, ethanol and the acetone at least
It is a kind of.
Wherein in some embodiments, the cosolvent is 10～50 μ L with the proportioning of the textile samples to be measured：1g.
Wherein in some embodiments, the cosolvent is methanol, the cosolvent and the textile samples to be measured
Proportioning is 45～50 μ L：1g.
Wherein in some embodiments, the organic solvent selected from normal hexane, ethyl acetate, carbon tetrachloride, hexamethylene and
At least one in toluene.
Wherein in some embodiments, the organic solvent is 1.2-1.8mL with the proportioning of the textile samples to be measured：
1g。
Wherein in some embodiments, the time of the shaking is 1-2 minutes.
Wherein in some embodiments, the mass fraction 0.8-1.2% of the solution of potassium carbonate, the solution of potassium carbonate with
The proportioning of the textile samples to be measured is 0.25-0.35mL：1g.
Wherein in some embodiments, the method for the phenol compound in the detection testing sample solution is GC-FID
Detection or GC-MS detections.
Wherein in some embodiments, the condition of the GC-FID detections is as follows：Chromatographic column be DB-624 (60m ×
0.32mm×1.8μm)；Injector temperature is 245-255 DEG C；Carrier gas is helium, and flow velocity is 0.9-1.1mL/min；Fid detector
Temperature is 275-285 DEG C；Sample size is 0.8-1.2 μ L；
The condition of the GC-MS detections is as follows：Chromatographic column is DB-17MS (30m × 0.25mm × 0.1 μm)；Injection port temperature
Spend for 265-275 DEG C；Chromatography-mass spectroscopy interface temperature is 255-265 DEG C；Carrier gas is helium, and flow velocity is 1.1-1.3mL/min；Electricity
It is EI from mode；Ionization energy is 65-75eV；Ion source temperature is 225-235 DEG C；Test mode is Selected ion monitoring mode；
Sample size is 0.8-1.2 μ L.
Wherein in some embodiments, the phenol compound is pentachlorophenol, tetrachlorophenol, trichlorophenol, 2,4,6,-T, dichloro
Phenol, monochloro phenol and o-phenyl phenol.
Supercritical fluid extraction is the new and high technology occurred in modern age chemical separating, and SFE is by traditional distillation and organic molten
Agent extraction integrally combines, using supercritical CO2Substrate and extract are efficiently separated, are extracted and purification by excellent solvent power.
SFE uses supercritical CO2Material is extracted, supercritical CO2It is safe and nontoxic and cheap liquid, which has similar gas
Diffusion coefficient, the dissolving power of liquid, surface tension is zero, among solid matter being penetrated into rapidly, with efficiently, be difficult oxygen
Change, pure natural, without the features such as chemical contamination.Supercritical fluid extraction isolation technics be using supercritical fluid solvability with
Its density is closely related, the density of supercritical fluid is significantly changed by changing pressure or temperature, in the supercritical state, will
Supercritical fluid is contacted with material to be separated so as to selectively successively polarity size, boiling point height and average molecular
Quality composition of different sizes is extracted.
The present inventor passes through lot of experiments, by supercritical CO2Abstraction technique is applied to phenol in textile
The extraction of class compound, and the phenol compound to extracting carries out derivatization in situ, through the simple extraction and derivatization
Pre-treatment after, you can carry out follow-up detection and analysis, you can realize phenol compound in textile sharp separation detection.
The method of detection and analysis can be gas chromatography-mass spectrum (GC-MS) separation detection or gas chromatogram separation detection.
The method for separating and detecting of phenol compound in the textile of the present invention, its pretreatment process solvent load are few, green
Colour circle is protected, and has quick, favorable reproducibility, simple operation and other advantages, overcomes traditional method not only time-consuming but also pollute lacking for environment
Fall into.And the method for the present invention can detect various containing chlorophenol and o-phenyl phenol simultaneously, the response rate of each phenol compound is high,
Between 85%～106%.
Description of the drawings
Fig. 1 is supercritical carbon dioxide extraction flow chart；
GC-MS total ion current figures of the Fig. 2 for 20 kinds of oxybenzene compounds in the textile samples of embodiment 1；
GC-FID chromatograms of the Fig. 3 for 20 kinds of oxybenzene compounds in the textile samples of embodiment 1.
Specific embodiment
Below by way of specific embodiment, the invention will be further described, but this is not limitation of the present invention.
Embodiment 1
10g textile samples are added in extraction kettle (supercritical carbon dioxide extraction flow chart is referring to Fig. 1), are added
Cosolvent-the methanol of 500 μ L acetic anhydrides and 500 μ L, it is 35MPa to set extraction temperature as 50 DEG C, pressure, is filled with 30mL supercritical
CO2Textile samples are carried out with supercritical carbon dioxide static extracting 10min；Extract with Pressure behaviour at the same temperatures again
15min, supercritical CO2Flow velocity 2.0mL/min；Outlet valve is opened, the object for extracting is separated and collected in device cooling
15mL n-hexane dissolutions are used, the solution of potassium carbonate that 3mL mass fractions are 1% is added in extract, 1min, normal hexane phase Jing is shaken
1g anhydrous sodium sulfate dehydrations, obtain testing sample solution；With gas chromatograph-mass spectrometer (GC-MS) (GC-MS) or gas chromatograph (GC-
FID) testing sample solution is carried out qualitative and quantitative analysis.
GC-MS test conditions are as follows：
Chromatographic column：DB-17MS(30m×0.25mm×0.1μm)；Heating schedule：50 DEG C (2min) are raised to 30 DEG C/min
220 DEG C (1min), then 260 DEG C (1min) are raised to 6 DEG C/min；Injector temperature：270℃；Chromatography-mass spectroscopy interface temperature：260
℃；Carrier gas：Helium, purity >=99.999%, flow 1.2mL/min；Ionization mode：EI；Ionization energy：70eV；Ion source temperature：
230℃；Test mode：Selected ion monitoring mode；Input mode：Splitless injecting-Sample；Sampling volume：1μL；Solvent delay：
1.2min。
GC-FID test conditions are as follows：
Chromatographic column：DB-624(60m×0.32mm×1.8μm)；Injector temperature：250℃；Carrier gas：Helium, purity >=
99.999%, flow velocity 1.0mL/min；Fid detector temperature：280℃；Heating schedule：60 DEG C of initial temperature, keeps 2min, with 8
DEG C/min is raised to 150 DEG C, is finally raised to 220 DEG C with 15 DEG C/min, keeps 8min；Sample size：1μL；Input mode：It is not diverted into
Sample；Hydrogen flowing quantity：40.0mL/min, air mass flow：450.0mL/min, make-up gas flow：50.0mL/min.
GC-MS detection total ion current figure as shown in Fig. 2 wherein, 1:2- chlorophenols, 2:3- chlorophenols, 3:4- chlorophenols,
4:2,6- chlorophenesic acids, 5:2,4- chlorophenesic acids, 2,5- chlorophenesic acids, 6:3,5- chlorophenesic acids, 7:2,3- chlorophenesic acids, 8:3,
4- chlorophenesic acids, 9:2,4,6- trichlorophenol, 2,4,6,-Ts, 10:2,3,6- trichlorophenol, 2,4,6,-Ts, 11:2,3,5- trichlorophenol, 2,4,6,-Ts, 12:2,4,5- trichlorines
Phenol, 13:2,3,4- trichlorophenol, 2,4,6,-Ts, 14:3,4,5- trichlorophenol, 2,4,6,-Ts, 15:O-phenyl phenol, 16:2,3,5,6- tetrachlorophenols,
17:2,3,4,6- tetrachlorophenols, 18:2,3,4,5- tetrachlorophenols, 19:Pentachlorophenol.
GC-FID detection chromatogram as shown in figure 3, wherein, 1:2- chlorophenols, 2:3- chlorophenols, 3:4- chlorophenols, 4:
2,6- chlorophenesic acids, 5:2,4- chlorophenesic acids, 2,5- chlorophenesic acids, 6:3,5- chlorophenesic acids, 7:2,3- chlorophenesic acids, 8:3,4-
Chlorophenesic acid, 9:2,4,6- trichlorophenol, 2,4,6,-Ts, 10:2,3,6- trichlorophenol, 2,4,6,-Ts, 11:2,3,5- trichlorophenol, 2,4,6,-Ts, 12:2,4,5- trichloro-benzenes
Phenol, 13:2,3,4- trichlorophenol, 2,4,6,-Ts, 1:4:3,4,5- trichlorophenol, 2,4,6,-Ts, 15：O-phenyl phenol, 16:2,3,5,6- tetrachlorophenols, 17:
2,3,4,6- tetrachlorophenols, 18:2,3,4,5- tetrachlorophenols, 19:Pentachlorophenol.
Embodiment 2
10g textile samples are added in extraction kettle, add the cosolvent-dichloromethane of 500 μ L acetic anhydrides and 500 μ L
Alkane, it is 40MPa to set extraction temperature as 50 DEG C, pressure, is filled with 30mL supercritical COs2Supercritical dioxy is carried out to textile samples
Change carbon static extracting 5min；20min, supercritical CO are extracted with Pressure behaviour at the same temperatures again2Flow velocity 1.2mL/min；
Open outlet valve, the object for extracting separating and collecting in device with the dissolving of 15mL toluene, addition 3mL matter in extract in cooling
Amount fraction is 1% solution of potassium carbonate, shakes 1min, and toluene phase Jing 1g anhydrous sodium sulfate dehydrations obtain testing sample solution；With
GC-MS or GC-FID carry out qualitative and quantitative analysis to testing sample solution.The same embodiment of test condition of GC-MS and GC-FID
1。
Embodiment 3
10g textile samples are added in extraction kettle, add the cosolvent-acetone of 500 μ L acetic anhydrides and 500 μ L, if
Determine extraction temperature be 70 DEG C, pressure be 30MPa, the flow velocity of supercritical carbon dioxide be 8.0mL/min, textile samples are carried out
Supercritical carbon dioxide dynamic extraction 30min；15mL ethyl acetate is added in collection device, outlet valve is opened, is collected and is separated out
Thing, adds the solution of potassium carbonate that 3mL mass fractions are 1%, shakes 1min, the anhydrous sulfur of ethyl acetate phase Jing 1g in extract solution
Sour sodium dehydration, obtains testing sample solution；Testing sample solution is carried out qualitative and quantitative analysis with GC-MS or GC-FID.GC-MS
With the test condition of GC-FID with embodiment 1.
Embodiment 4
10g textile samples are added in extraction kettle, add the cosolvent-benzene of 500 μ L acetic anhydrides and 500 μ L, setting
Extraction temperature is 60 DEG C, pressure is 40MPa, is filled with 30mL supercritical COs2Supercritical carbon dioxide is carried out to textile samples quiet
State extracts 10min；15min, supercritical CO are extracted with Pressure behaviour at the same temperatures again2Flow velocity 6mL/min；Open discharging
Valve, the object for extracting separating and collecting in device with the dissolving of 15mL hexamethylene, addition 3mL mass fractions in extract in cooling
For 1% solution of potassium carbonate, 1min is shaken, hexamethylene phase Jing 1g anhydrous sodium sulfate dehydrations obtain testing sample solution；Use GC-MS
Or GC-FID carries out qualitative and quantitative analysis to testing sample solution.The test condition of GC-MS and GC-FID is with embodiment 1.
Embodiment 5
10g textile samples are added in extraction kettle, add the cosolvent-ethanol of 500 μ L acetic anhydrides and 500 μ L, if
It is 45MPa to determine extraction temperature for 40 DEG C, pressure, is filled with 30mL supercritical COs2Supercritical carbon dioxide is carried out to textile samples
Static extracting 15min；20min, supercritical CO are extracted with Pressure behaviour at the same temperatures again2Flow velocity 3.0mL/min；Open
Outlet valve, the object for extracting separating and collecting in device with the dissolving of 15mL carbon tetrachloride, addition 3mL matter in extract in cooling
Amount fraction is 1% solution of potassium carbonate, shakes 1min, and carbon tetrachloride phase Jing 1g anhydrous sodium sulfate dehydrations obtain testing sample solution；
Testing sample solution is carried out qualitative and quantitative analysis with GC-MS or GC-FID.The test condition of GC-MS and GC-FID is with enforcement
Example 1.
Embodiment 6
10g textile samples are added in extraction kettle, add 500 μ L acetic anhydrides (without cosolvent), setting extraction
Temperature is 80 DEG C, pressure is 15MPa, is filled with 30mL supercritical COs2Textile samples are carried out with the static extraction of supercritical carbon dioxide
Take 20min；15min, supercritical CO are extracted with Pressure behaviour at the same temperatures again2Flow velocity 5.0mL/min；Open discharging
Valve, the object for extracting separating and collecting in device with the dissolving of 15mL hexamethylene, addition 3mL mass fractions in extract in cooling
For 1% solution of potassium carbonate, 1min is shaken, hexamethylene phase Jing 1g anhydrous sodium sulfate dehydrations obtain testing sample solution；Use GC-MS
Or GC-FID carries out qualitative and quantitative analysis to testing sample solution.The test condition of GC-MS and GC-FID is with embodiment 1.
The test of 7 response rate of embodiment
Method of testing is as follows：Take 10g blank textile samples, the mixed mark of addition phenol compound, every kind of compound addition
Amount is 10mg (taking the mixed mark of phenol compound that 10mL concentration is 1000mg/L), after solvent is evaporated completely, obtains response rate survey
Test agent, is carried out extracting to response rate test sample by the condition in embodiment 1-6, derivatization in situ, GC-MS or GC- respectively
FID is detected.Response rate test result is as shown in table 1.
The response rate (%) of 20 kinds of phenol compounds of 1 embodiment 1-6 of table
Standard GB/T/T 18414.2-2006《The measure part 2 of textile chlorinated phenol：Gas chromatography》In it is whole
Individual method of testing is as follows：1.0g textile samples carry out supersound extraction (each 20mL ultrasounds 15min) 3 times using acetone point, extract
Liquid is rotated after merging near dry, is dissolved in three times and is transferred in separatory funnel with 30mL solution of potassium carbonate (0.1mol/L), plus
After entering 1mL acetic anhydrides shaking 2min, 5.0mL normal hexane is added, then shakes 2min, stood 5min, discard lower floor, normal hexane is mutually used
20g/L metabisulfite solutions wash 2 times (each consumption 20mL), and lower floor, upper liquid Jing about 1.0g anhydrous slufuric acids are discarded after stratification
After sodium dehydration, for gas chromatograph for determination.In the national standard, 1.0g textile samples use organic solvent：60mL acetone, 5mL are just
Hexane and 1mL acetic anhydrides, whole pre-treatment take at least 60min.
And the method for separating and detecting of the present invention avoids the deficiencies such as the time-consuming consumptive material of traditional method (national standard), at 30 points
Clock interior energy separates ten several above oxybenzene compounds.The method for separating and detecting of the present invention, its pre-treatment are quick, environmental protection, flow process letter
It is single, and favorable reproducibility, it is used in conjunction with gas chromatograph, gas chromatograph-mass spectrometer (GC-MS), you can realize phenol in textile
The sharp separation detection of compound, can detect various containing chlorophenol and o-phenyl phenol simultaneously, and the response rate of each phenol compound is high,
Between 85%～106%.
Each technical characteristic of embodiment described above arbitrarily can be combined, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more concrete and detailed, but and
Therefore can not be construed as limiting the scope of the patent.It should be pointed out that for one of ordinary skill in the art comes
Say, without departing from the inventive concept of the premise, some deformations and improvement can also be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be defined by claims.
Claims (10)
1. in a kind of textile phenol compound method for separating and detecting, it is characterised in that comprise the following steps：
Take textile samples to be measured to be added in extraction kettle, add derivatization reagent or addition derivatization reagent and cosolvent,
Textile samples to be measured are carried out with supercritical carbon dioxide extraction, collection obtains extract；The supercritical carbon dioxide extraction
Temperature be 40～90 DEG C, pressure be 15～45MPa；
Extract organic solvent is dissolved, extract solution is obtained, solution of potassium carbonate is added, shaking, organic faciess are dry with desiccant
It is dry, obtain testing sample solution；
Phenol compound in detection testing sample solution.
2. in textile according to claim 1 phenol compound method for separating and detecting, it is characterised in that it is described super
The process of critical carbon dioxide extraction is 25～40min of dynamic extraction or 5～30min of first static extracting, then dynamic extraction 10
～20min；During static extracting, the supercritical carbon dioxide is 2-4mL with the proportioning of the textile samples to be measured：1g；It is dynamic
When state is extracted, the flow velocity of the supercritical carbon dioxide is 1～10mL/min.
3. in textile according to claim 1 and 2 phenol compound method for separating and detecting, it is characterised in that institute
It is acetic anhydride to state derivatization reagent, and the derivatization reagent is 10～50 μ L with the proportioning of the textile samples to be measured：1g.
4. in textile according to claim 1 and 2 phenol compound method for separating and detecting, it is characterised in that institute
State at least one of the cosolvent in benzene, dichloromethane, methanol, ethanol and acetone.
5. in textile according to claim 4 phenol compound detection method, it is characterised in that the cosolvent
Proportioning with the textile samples to be measured is 10～50 μ L：1g.
6. in textile according to claim 1 and 2 phenol compound method for separating and detecting, it is characterised in that institute
State at least one of the organic solvent in normal hexane, ethyl acetate, carbon tetrachloride, hexamethylene and toluene.
7. in textile according to claim 6 phenol compound method for separating and detecting, it is characterised in that it is described to have
Machine solvent is 1.2-1.8mL with the proportioning of the textile samples to be measured：1g.
8. in textile according to claim 1 and 2 phenol compound method for separating and detecting, it is characterised in that institute
The mass fraction 0.8-1.2% of solution of potassium carbonate is stated, the solution of potassium carbonate with the proportioning of the textile samples to be measured is
0.25-0.35mL：1g.
9. according to the method for separating and detecting of phenol compound in the textile described in claim 1 or 2, it is characterised in that described
The method of the phenol compound in detection testing sample solution is that GC-FID is detected or GC-MS detections.
10. according to the method for separating and detecting of phenol compound in the textile described in claim 1 or 2, it is characterised in that described
Phenol compound is pentachlorophenol, tetrachlorophenol, trichlorophenol, 2,4,6,-T, chlorophenesic acid, monochloro phenol and o-phenyl phenol.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108107132A (en) * | 2017-12-27 | 2018-06-01 | 福建出入境检验检疫局检验检疫技术中心 | The detection method of phenol total content in a kind of leather and its leather products |
| CN108107132B (en) * | 2017-12-27 | 2020-10-27 | 福建出入境检验检疫局检验检疫技术中心 | Method for detecting total content of phenol in leather and leather products thereof |
| CN109187782A (en) * | 2018-09-03 | 2019-01-11 | 必维申优质量技术服务江苏有限公司 | The novel detection method of chlorophenol in textile |
| CN110568104A (en) * | 2019-09-24 | 2019-12-13 | 杭州市质量技术监督检测院 | Method for simultaneously measuring migration volumes of various chlorinated phenols in wooden tableware |
| CN111257489A (en) * | 2020-01-21 | 2020-06-09 | 浙江工业大学 | Method for analyzing volatile phenolic compounds in water based on ultrasonic-assisted in-situ bubbling and simultaneous derivatization-dispersion liquid-liquid microextraction |
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