CN106645448B - The method for separating and detecting of phenol compound in textile - Google Patents
The method for separating and detecting of phenol compound in textile Download PDFInfo
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Abstract
The present invention relates to a kind of method for separating and detecting of phenol compound in textile, the following steps are included: textile samples to be measured is taken to be added in extraction kettle, add derivatization reagent or addition derivatization reagent and cosolvent, supercritical carbon dioxide extracting is carried out to textile samples to be measured, collection obtains extract；The temperature of the supercritical carbon dioxide extracting is 40~90 DEG C, and pressure is 15~45MPa；Extract is dissolved with organic solvent, obtains extract solution, solution of potassium carbonate, shaking is added, organic phase desiccant dryness obtains testing sample solution；Detect the phenol compound in testing sample solution.The method for separating and detecting of phenol compound in textile of the invention, its pretreatment process solvent usage is few, environmentally protective, and has quick, favorable reproducibility, simple operation and other advantages, and it can detect simultaneously various containing chlorophenol and o-phenyl phenol, the rate of recovery height of each phenol compound.
Description
Technical field
The present invention relates to textile and analysis detection fields, more particularly to phenol compound in a kind of textile
Method for separating and detecting.
Background technique
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 fungicide and preservative.These compounds all have certain bio-toxicity effect, can be to environment and people
Body health has an impact, and therefore, the residue problem in textiles and leathers is concerned.As related toxicity and toxicity are ground
That studies carefully deepens continuously, and relevant law, regulation and standard have stringent limitation to its residue limits in textile.Germany is right
The limitation requirement of TeCP and PCP: product in direct contact with the skin is 0.05mg/kg, and product not in direct contact with the skin is
5mg/kg；Limitation requirement of the France to PCP: product in direct contact with the skin is 0.5mg/kg, not in direct contact with the skin
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 product
It is 0.5mg/kg in I class product that kg, which is 2.0mg/kg, DCP and MCP in II class, III class and IV class product, II class, III class and
It is 3.0mg/kg in IV class product, OPP is 50.0mg/kg in I class product, is in II class, III class and IV class product
100.0mg/kg.China standard GB/T 18885-2009 has also carried out stringent limitation to PCP, TeCP and OPP.
Currently, main method of the measurement containing chlorophenol, o-phenyl phenol is by Soxhlet extraction, ultrasonic extraction or to add both at home and abroad
It after quick-dissolving agent extracts, performs the derivatization, then uses gas-chromatography-electron capture detector (ECD) (GC-ECD) or gas-chromatography-quality
Select detector (GC-MS) measurement.These technologies have the defects that detect simultaneously it is various containing chlorophenol and o-phenyl phenol, and
There is the defects of time-consuming, organic solvent usage amount is big.
Summary of the invention
Based on this, the present invention provides a kind of method for separating and detecting of phenol compound in textile, the detection methods
Have the advantages that quick, solvent usage is few, environmentally protective.
Specific technical solution is as follows:
The method for separating and detecting of phenol compound in a kind of textile, comprising the following steps:
It takes textile samples to be measured to be added in extraction kettle, add derivatization reagent or addition derivatization reagent and is total to molten
Agent carries out supercritical carbon dioxide extracting to textile samples to be measured, and collection obtains extract；The supercritical carbon dioxide extraction
The temperature taken is 40~90 DEG C, and pressure is 15~45MPa；
Extract is dissolved with organic solvent, obtains extract solution, solution of potassium carbonate, shaking, organic phase drying is added
Agent is dry, obtains testing sample solution；
Detect the phenol compound in testing sample solution.
In wherein some embodiments, the process of the supercritical carbon dioxide extracting be 25~40min of dynamic extraction or
Person elder generation 5~30min of static extracting, then 10~20min of dynamic extraction；When static extracting, the supercritical carbon dioxide with it is described
The proportion of textile samples to be measured is 2-4mL:1g；When dynamic extraction, the flow velocity of the supercritical carbon dioxide is 1~10mL/
min。
In wherein some embodiments, the process of the supercritical carbon dioxide extracting is 8~15min of first static extracting,
10~20min of dynamic extraction again；When dynamic extraction, the flow velocity of the supercritical carbon dioxide is 1.5~2.5mL/min.
In wherein some embodiments, the temperature of the supercritical carbon dioxide extracting is 45~55 DEG C, pressure is 30~
40MPa。
In wherein some embodiments, the derivatization reagent is acetic anhydride, the derivatization reagent and the spinning to be measured
The proportion of fabric sample is 10~50 μ L:1g.
In wherein some embodiments, the proportion of the derivatization reagent and the textile samples to be measured is 45~50 μ
L:1g.
In wherein some embodiments, the cosolvent in benzene, methylene chloride, methanol, ethyl alcohol and acetone at least
It is a kind of.
In wherein some embodiments, the proportion of the cosolvent and the textile samples to be measured is 10~50 μ L:1g.
In wherein some embodiments, the cosolvent is methanol, the cosolvent and the textile samples to be measured
Proportion is 45~50 μ L:1g.
In wherein some embodiments, the organic solvent be selected from n-hexane, ethyl acetate, carbon tetrachloride, hexamethylene and
At least one of toluene.
In wherein some embodiments, the proportion of the organic solvent and the textile samples to be measured is 1.2-1.8mL:
1g。
In wherein some embodiments, the time of the shaking is 1-2 minutes.
In wherein some embodiments, the mass fraction 0.8-1.2% of the solution of potassium carbonate, the solution of potassium carbonate with
The proportion of the textile samples to be measured is 0.25-0.35mL:1g.
In wherein some embodiments, the method for the phenol compound in the detection testing sample solution is GC-FID
Detection or GC-MS detection.
In wherein some embodiments, the condition of GC-FID detection be as follows: chromatographic column for DB-624 (60m ×
0.32mm×1.8μm)；Injector temperature is 245-255 DEG C；Carrier gas is helium, flow velocity 0.9-1.1mL/min；Fid detector
Temperature is 275-285 DEG C；Sample volume is 0.8-1.2 μ L；
The condition of the GC-MS detection is as follows: chromatographic column is DB-17MS (30m × 0.25mm × 0.1 μm)；Injection port temperature
Degree is 265-275 DEG C；Chromatography-mass spectroscopy interface temperature is 255-265 DEG C；Carrier gas is helium, flow velocity 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 volume is 0.8-1.2 μ L.
In wherein 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, and utilizes supercritical CO2Matrix is efficiently separated, extracted and purified with extract by excellent solvent power.
SFE uses supercritical CO2Material is extracted, supercritical CO2It is safe and nontoxic and cheap liquid, there is similar gas
Diffusion coefficient, liquid dissolving power, surface tension zero can penetrate among solid matter rapidly, have efficiently, be not easy oxygen
The features such as changing, be pure natural, without chemical contamination.Supercritical fluid extraction isolation technics be using supercritical fluid solvability with
Its density is closely related, changes the density of supercritical fluid substantially by changing pressure or temperature, in the supercritical state, will
Supercritical fluid is in contact with the substance to be separated, and makes it selectively successively polarity size, boiling point height and average molecular
Quality ingredient of different sizes extracts.
The present inventor is by lot of experiments, by supercritical CO2Abstraction technique is applied to phenol in textile
The extraction of class compound, and derivatization in situ is carried out to the phenol compound of extraction, by the simple extraction and derivatization
Pre-treatment after, subsequent detection and analysis can be carried out, can be realized phenol compound in textile quick separating detection.
The method of detection and analysis can be gas chromatography-mass spectrum (GC-MS) separation detection or gas-chromatography separation detection.
The method for separating and detecting of phenol compound in textile of the invention, pretreatment process solvent usage is few, green
Colour circle protect, and have quickly, favorable reproducibility, simple operation and other advantages, overcome conventional method it is not only time-consuming but also pollute environment lack
It falls into.And method of the invention can detect various containing chlorophenol and o-phenyl phenol simultaneously, and the rate of recovery of each phenol compound is high,
Between 85%~106%.
Detailed description of the invention
Fig. 1 is supercritical carbon dioxide extracting flow chart；
Fig. 2 is the GC-MS total ion current figure of 20 kinds of oxybenzene compounds in the textile samples of embodiment 1；
Fig. 3 is the GC-FID chromatogram of 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 a limitation of the present invention.
Embodiment 1
10g textile samples are added in extraction kettle (supercritical carbon dioxide extracting flow chart is referring to Fig. 1), are added
Cosolvent-methanol of 500 μ L acetic anhydrides and 500 μ L sets extraction temperature as 50 DEG C, pressure 35MPa, it is overcritical to be filled with 30mL
CO2Supercritical carbon dioxide static extracting 10min is carried out to textile samples；It is extracted at the same temperatures with Pressure behaviour again
15min, supercritical CO2Flow velocity 2.0mL/min；Outlet valve is opened, the object extracted separates and collects in device in cooling
The solution of potassium carbonate that 3mL mass fraction is 1% is added with 15mL n-hexane dissolution, in extract liquor, shakes 1min, n-hexane mutually passes through
The dehydration of 1g anhydrous sodium sulfate, obtains testing sample solution；With gas chromatograph-mass spectrometer (GC-MS) (GC-MS) or gas chromatograph (GC-
FID it) carries out qualitative and quantitative analysis to testing sample solution.
GC-MS test condition is as follows:
Chromatographic column: DB-17MS (30m × 0.25mm × 0.1 μm)；Temperature program: 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 DEG C；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: 1 μ L；Solvent delay:
1.2min。
GC-FID test condition is as follows:
Chromatographic column: DB-624 (60m × 0.32mm × 1.8 μm)；Injector temperature: 250 DEG C；Carrier gas: helium, purity >=
99.999%, flow velocity 1.0mL/min；Fid detector temperature: 280 DEG C；Temperature program: 60 DEG C of initial temperature, 2min is kept, with 8
DEG C/min is raised to 150 DEG C, is finally raised to 220 DEG C with 15 DEG C/min, keep 8min；Sample volume: 1 μ L；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.
The total ion current figure of GC-MS detection is as shown in Figure 2, wherein 1:2- chlorophenol, 2:3- chlorophenol, and 3:4- chlorophenol,
4:2,6- chlorophenesic acid, 5:2,4- chlorophenesic acid, 2,5- chlorophenesic acid, 6:3,5- chlorophenesic acid, 7:2,3- chlorophenesic acid, 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- 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.
The chromatogram of GC-FID detection is as shown in Figure 3, wherein 1:2- chlorophenol, 2:3- chlorophenol, and 3:4- chlorophenol, 4:
2,6- chlorophenesic acids, 5:2,4- chlorophenesic acid, 2,5- chlorophenesic acid, 6:3,5- chlorophenesic acid, 7:2,3- chlorophenesic acid, 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, 500 μ L acetic anhydrides and cosolvent-dichloromethane of 500 μ L are added
Alkane sets extraction temperature as 50 DEG C, pressure 40MPa, is filled with 30mL supercritical CO2Overcritical 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；
Outlet valve is opened, the object extracted is dissolved in cooling separating and collecting in device with 15mL toluene, and 3mL matter is added in extract liquor
The solution of potassium carbonate that score is 1% is measured, 1min is shaken, toluene is mutually dehydrated through 1g anhydrous sodium sulfate, obtains testing sample solution；With
GC-MS or GC-FID carry out qualitative and quantitative analysis to testing sample solution.The same embodiment of the test condition of GC-MS and GC-FID
1。
Embodiment 3
10g textile samples are added in extraction kettle, 500 μ L acetic anhydrides and cosolvent-acetone of 500 μ L are added, if
Determine that extraction temperature is 70 DEG C, the flow velocity of pressure 30MPa, supercritical carbon dioxide is 8.0mL/min, textile samples are carried out
Supercritical carbon dioxide dynamic extraction 30min；15mL ethyl acetate is added in collection device, opens outlet valve, collects and is precipitated
The solution of potassium carbonate that 3mL mass fraction is 1% is added in extract solution, shakes 1min, ethyl acetate phase is through the anhydrous sulphur of 1g for object
Sour sodium dehydration, obtains testing sample solution；It is carried out qualitative and quantitative analysis with GC-MS or GC-FID to testing sample solution.GC-MS
Test condition with GC-FID is the same as embodiment 1.
Embodiment 4
10g textile samples are added in extraction kettle, 500 μ L acetic anhydrides and cosolvent-benzene of 500 μ L, setting are added
Extraction temperature is 60 DEG C, pressure 40MPa, is filled with 30mL supercritical CO2It is quiet that supercritical carbon dioxide is carried out to textile samples
State extracts 10min；15min, supercritical CO are extracted with Pressure behaviour at the same temperatures again2Flow velocity 6mL/min；Open discharging
Valve, the object extracted are dissolved in cooling separating and collecting in device with 15mL hexamethylene, and 3mL mass fraction is added in extract liquor
For 1% solution of potassium carbonate, 1min is shaken, hexamethylene is mutually dehydrated through 1g anhydrous sodium sulfate, obtains 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 the same as embodiment 1.
Embodiment 5
10g textile samples are added in extraction kettle, 500 μ L acetic anhydrides and cosolvent-ethyl alcohol of 500 μ L are added, if
Determine extraction temperature be 40 DEG C, pressure 45MPa, be filled with 30mL supercritical CO2Supercritical 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；It opens
Outlet valve, the object extracted are dissolved in cooling separating and collecting in device with 15mL carbon tetrachloride, and 3mL matter is added in extract liquor
The solution of potassium carbonate that score is 1% is measured, 1min is shaken, carbon tetrachloride is mutually dehydrated through 1g anhydrous sodium sulfate, obtains testing sample solution；
It is carried out qualitative and quantitative analysis with GC-MS or GC-FID to testing sample solution.The test condition of GC-MS and GC-FID is the same as implementation
Example 1.
Embodiment 6
10g textile samples are added in extraction kettle, 500 μ L acetic anhydrides (not adding cosolvent), setting extraction are added
Temperature is 80 DEG C, pressure 15MPa, is filled with 30mL supercritical CO2Supercritical carbon dioxide static state extraction is carried out to textile samples
Take 20min；15min, supercritical CO are extracted with Pressure behaviour at the same temperatures again2Flow velocity 5.0mL/min；Open discharging
Valve, the object extracted are dissolved in cooling separating and collecting in device with 15mL hexamethylene, and 3mL mass fraction is added in extract liquor
For 1% solution of potassium carbonate, 1min is shaken, hexamethylene is mutually dehydrated through 1g anhydrous sodium sulfate, obtains 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 the same as embodiment 1.
The test of 7 rate of recovery of embodiment
Test method is as follows: taking 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 rate of recovery survey
Test agent respectively extracts rate of recovery test sample by the condition in embodiment 1-6, derivatization, GC-MS or GC- in situ
FID detection.Rate of recovery test result is as shown in table 1.
The rate of recovery (%) of 20 kinds of phenol compounds of 1 embodiment 1-6 of table
It is whole in standard GB/T/T 18414.2-2006 " the measurement part 2 of textile chlorinated phenol: gas chromatography "
A test method is as follows: 1.0g textile sample is extracted using 3 progress ultrasonic extractions (each 20mL ultrasound 15min) of acetone point
Liquid merges back spin and is steamed near dry, and is dissolved and is transferred in separatory funnel in three times with 30mL solution of potassium carbonate (0.1mol/L), added
After entering 1mL acetic anhydride shaking 2min, 5.0mL n-hexane is added, then shake 2min, stands 5min, discard lower layer, n-hexane is mutually used
20g/L metabisulfite solution is washed 2 times (each dosage 20mL), lower layer is discarded after stratification, upper liquid is through about 1.0g anhydrous slufuric acid
After sodium dehydration, for gas chromatograph for determination.1.0g textile sample uses organic solvent in the national standard: 60mL acetone, 5mL are just
Hexane and 1mL acetic anhydride, entire pre-treatment time-consuming at least 60min.
And method for separating and detecting of the invention avoids the deficiencies of conventional method (national standard) time-consuming consumptive material, at 30 points
Ten several above oxybenzene compounds can be separated in clock.Method for separating and detecting of the invention, pre-treatment is quick, environmental protection, process letter
It is single, and favorable reproducibility, it is used in conjunction with gas chromatograph, gas chromatograph-mass spectrometer (GC-MS), phenol in textile can be realized
The quick separating detection for closing object, can detect various containing chlorophenol and o-phenyl phenol simultaneously, and the rate of recovery of each phenol compound is high,
Between 85%~106%.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies 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, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. the method for separating and detecting of phenol compound in a kind of textile, which comprises the following steps:
It takes textile samples to be measured to be added in extraction kettle, adds derivatization reagent or addition derivatization reagent and cosolvent,
Supercritical carbon dioxide extracting is carried out to textile samples to be measured, collection obtains extract；The supercritical carbon dioxide extracting
Temperature be 45~55 DEG C, pressure be 30~40MPa；The process of the supercritical carbon dioxide extracting be dynamic extraction 25~
5~30min of 40min or first static extracting, then 10~20min of dynamic extraction；When static extracting, the supercritical carbon dioxide
Proportion with the textile samples to be measured is 2-4mL:1g；
Extract is dissolved with organic solvent, obtains extract solution, solution of potassium carbonate, shaking is added, organic phase is done with desiccant
It is dry, obtain testing sample solution；
The phenol compound in the testing sample solution is detected with GC-MS or GC-FID；
The GC-MS test condition is as follows:
Chromatographic column: DB-17MS；Temperature program: in 50 DEG C of holding 2min, being then raised to 220 DEG C with 30 DEG C/min, keep 1min,
260 DEG C are raised to 6 DEG C/min again, keeps 1min；Injector temperature: 270 DEG C；Chromatography-mass spectroscopy interface temperature: 260 DEG C；Carrier gas:
Helium, purity >=99.999%, flow 1.2mL/min；Ionization mode: EI；Ionization energy: 70eV；Ion source temperature: 230 DEG C；It surveys
Examination mode: Selected ion monitoring mode；Input mode: Splitless injecting-Sample；Sampling volume: 1 μ L；Solvent delay: 1.2min；
The GC-FID test condition is as follows:
Chromatographic column: DB-624；Injector temperature: 250 DEG C；Carrier gas: helium, purity >=99.999%, flow velocity 1.0mL/min；FID
Detector temperature: 280 DEG C；Temperature program: 60 DEG C of initial temperature, 2min is kept, 150 DEG C are raised to 8 DEG C/min, finally with 15
DEG C/min is raised to 220 DEG C, keep 8min；Sample volume: 1 μ L；Input mode: Splitless injecting samples；Hydrogen flowing quantity: 40.0mL/min,
Air mass flow: 450.0mL/min, make-up gas flow: 50.0mL/min；
The phenol compound is 2- chlorophenol, 3- chlorophenol, 4- chlorophenol, 2,3- chlorophenesic acid, o-phenyl phenol, 2,4-
Chlorophenesic acid, 2,5- chlorophenesic acid, 2,6- chlorophenesic acid, 3,4- chlorophenesic acid, 3,5- chlorophenesic acid, 2,3,4- trichlorophenol, 2,4,6,-T,
2,3,5- trichlorophenol, 2,4,6,-T, 2,3,6- trichlorophenol, 2,4,6,-T, 2,4,5- trichlorophenol, 2,4,6,-T, 2,4,6- trichlorophenol, 2,4,6,-T, 3,4,5- trichlorophenol, 2,4,6,-T, 2,
3,4,5- tetrachlorophenol, 2,3,4,6- tetrachlorophenol, 2,3,5,6- tetrachlorophenol and pentachlorophenol；
The derivatization reagent is acetic anhydride.
2. the method for separating and detecting of phenol compound in textile according to claim 1, which is characterized in that described to spread out
Biochemical reagents are acetic anhydride, and the proportion of the derivatization reagent and the textile samples to be measured is 10~50 μ L:1g.
3. the method for separating and detecting of phenol compound in textile according to claim 1, which is characterized in that described total
Solvent is selected from least one of benzene, methylene chloride, methanol, ethyl alcohol and acetone.
4. the detection method of phenol compound in textile according to claim 3, which is characterized in that the cosolvent
Proportion with the textile samples to be measured is 10~50 μ L:1g.
5. the method for separating and detecting of phenol compound in textile according to claim 1, which is characterized in that described to have
Solvent is selected from least one of n-hexane, ethyl acetate, carbon tetrachloride, hexamethylene and toluene.
6. the method for separating and detecting of phenol compound in textile according to claim 5, which is characterized in that described to have
The proportion of solvent and the textile samples to be measured is 1.2-1.8mL:1g.
7. the method for separating and detecting of phenol compound in textile according to claim 1, which is characterized in that the carbon
The proportion of the mass fraction 0.8-1.2% of sour potassium solution, the solution of potassium carbonate and the textile samples to be measured is 0.25-
0.35mL:1g.
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| 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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