CN105842376A - Method for detecting polychlorobiphenyl in dye - Google Patents
Method for detecting polychlorobiphenyl in dye Download PDFInfo
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- G—PHYSICS
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- 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
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
The invention discloses a method for detecting polychlorobiphenyl in dye. The method includes the steps that a dye sample to be detected is acetylated with acetic anhydride, and then ultrasonic oscillation is carried out for even mixing; analyte is extracted with a mixed solvent with an internal standard substance added; the obtained analyte is purified with carbon powder, subjected to column chromatography, subjected to centrifugal separation and filtered with a filter screen with the pore diameter smaller than 0.22 micrometer, and a clarified sample is obtained; the content of polychlorobiphenyl in the clarified sample is measured through a gas chromatography-mass spectrometer. The analysis method can be implemented by adjusting the process regardless of dye types, the defect that no dye detection standard is available for monochlorphenol, dichlorophenol and trichlorophenol is overcome, and compared with a textile inspection method in the prior art, the detection effect is better. Extraction time consumed in the experiment process is shorter than that in the prior art; besides, little waste is generated in the extraction method, so that higher environmental friendliness is achieved.
Description
Technical field
The present invention relates to the detection method of harmful substance in a kind of dyestuff, be specifically related to the inspection of polystream phenol in a kind of dyestuff
Survey method.
Background technology
(being called for short: PCP), outward appearance is white flakes or crystalline solid, often the water of crystallization Han a part, the hottest have pentachlorophenol
Extremely strong pungent stink, pentachlorophenol is preservative common in the products such as textile, leather, timber, can be changed into two during burning
Dislike English class extremely toxic substance.Animal experiment proves that, PCP is the extremely toxic substance of biological carcinogenecity, and can accumulate in organism, makes
Become irreversible impact.
Tetrachlorophenol uses relatively broad on insecticide, and it is right also to have proposition in international cancer research institution (IARC)
Biological impact, though uncertain impact on human body, but also can not be ignored.And in 2016, global environmental protection tissue
Oeko TexStandard100 has also increased conventional unheeded chlorophenic acid and chlorophenesic acid in the keyholed back plate regulations of nuisance newly
Content limit.
Environmental protection specification limit was confined in finished product mostly in the past, and the most current detection method the most only terminates in textile (XP-
G08015) with the standard assays of leather (ISO17070).Further, about chlorophenic acid, chlorophenesic acid in leather and textile
Issue relevant criterion method is yet there are no Deng measuring while 9 kinds of isomerss and tetrachlorophenol and pentachlorophenol.Ring in recent years
Protect subject under discussion be gradually concerned, not only terminate in finished product, the nuisance composition of its raw material also starts emphatically, the People's Republic of China (PRC) in
The detection national standard promulgated for 2009 is also only restricted in tetrachlorophenol and the detection (GB/T24166-of pentachlorophenol in dyestuff
2009)。
The most conventional detection method has: ISO 17070:2006 " pentachlorophenol detection method of content in leather "；Country
Standard GB/T 18414.2-2006 " mensuration of textile chlorinated phenol "；Standard GB/T/T24166-2009 " chlorobenzene in dyestuff
The mensuration of phenol "；But above-mentioned detection method, have the following disadvantages: 1. at present technology to trichlorophenol, 2,4,6,-T, tetrachlorophenol and five
Chlorophenol, only for finished product detection, raw material result can there is any discrepancy in kind detection；2. currently for the technology of dyestuff extraction
Detection only for tetrachlorophenol Yu pentachlorophenol；Extraction dyestuff impurity is difficult to remove the most in a conventional method；The most existing dyestuff extracts
Chlorophenic acid, chlorophenesic acid are the highest with the degree of stability of trichlorophenol, 2,4,6,-T and solvent is to dyestuff problems of dissolution for extracting for access method set
The most perfect.
Summary of the invention
The technical problem to be solved is: provide one extraction amount of solution few, many in the dyestuff that waste liquid amount is relatively low
The detection method of chlorophenol, this detection method can overcome chlorophenic acid, chlorophenesic acid and trichlorophenol, 2,4,6,-T not to have dyestuff to detect
The defect of examination criteria.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: the detection of polystream phenol in a kind of dyestuff
Method, the steps include:
By dye sample to be measured through acetic anhydride acetylation, through sonic oscillation mix homogeneously, then divide with mixing solvent extraction
Analysis thing, then do purified treatment through carbon dust, column chromatography carries out purifying, centrifugation, < strainer filtering of 0.22 μm obtains clear in aperture
Final proof product, this clarification sample measures the content of polystream phenol and its derivant through gaseous mass analyzer, utilizes and selects ion and arrange in pairs or groups
External standard does numerical examination；
This analysis method is directed to the detection of polystream phenol and its derivant in dyestuff, and its sample recovery rate reaches 92-115%,
And its relative standard deviation of duplicate detection (Relative Standard Deviation, RSD)≤5.3% (sample number, N=
6)。
Described dye sample to be measured extracts and obtains clarifying concretely comprising the following steps of sample:
1) acetylation: mixed with acetic anhydride by dye sample to be measured, reduces in acetic anhydride and described dye sample to be measured
The mol ratio of group > 1, the sample mixed, through ultrasonic vibration at least 30min, treats that dyestuff is all as bottom；
2) extract: to ultrasonic complete after dye sample to be measured in add mixed solvent carry out dissolution extraction, it is desirable to dye to be measured
Material sample is formed homogeneously with mixed solvent, to guarantee fully to dissolve (according to different dyes structure, dispersant between dyestuff and solvent
Kind to the mixing time, add lysate adjust)；
Internal standard substance is added in extraction mixed solvent；Different solvents is individually added into identical purity be higher than
The internal standard substance of 99.9wt.%, remixes formation mixed solvent, and internal standard substance is 10 ± 0.05ppm at the content of mixed solvent；Described
The structure of internal standard substance close with polystream phenol, and can occur in detection temperature range, and not with testing sample, quench that it is molten to take
Agent reaction has influence on loss and the interference of extraction process；
Include the disperse dyes of water soluble dispersing agent, for guaranteeing that the uniformity that dyestuff dissolves must be added to 0.5mL-5mL's
The resistivity water more than 18M Ω * cm and disperse dyes effect, the most again with mixed solvent dissolution extraction；
3) purify: by step 2) homogeneous sample that the dye sample to be measured of gained is formed with mixed solvent, does through carbon dust
Purified treatment, purifies through column chromatography the most again, reduces the signal strength of impact analysis thing；
4) separate: by step 3) sample that gained purifies, the centrifuge with rotating speed as 2000-3500rpm is at least
5min, to guarantee that impurity is removed completely, < strainer filtering of 0.22 μm, gained defecation takes out, utilizes gas phase matter last via hole diameter
Spectrometer detects.
Described dye sample to be measured, the mixing solvent load used in extraction process is: every 0.5 ± 0.001mL liquid
Dye sample to be measured or 0.5 ± 0.0001g solid dye sample to be measured use 5 ± 0.005mL to mix solvent.
Described mixed solvent is two or more combination in normal hexane, toluene, isopropanol, acetone.
Described internal standard substance is four chlorination o-methoxyphenols.
Described carbon dust, purifies at least 1h with 300-400 DEG C before use.
The column chromatography filler used in described column chromatography procedure is silica gel or kieselguhr, the every 0.1-replacing deactivation
10g dye sample to be measured, with 1 ± 0.001g column chromatography filler.
Illustrate: each sample must add composition to be measured (internal standard method or external standard method) with determine this sample the response rate and
Detectable limit；There is the situation of the more interference of background value in determinand to sample, and causes the detection of the internal standard substance response rate to limit low
In the sample of 0.05ppm, need substrate purification process, but most of environment and the extraction of garbage sample, the most all
Need to process in advance；When sample interference value is higher than the situation of measured object or causes retention time to offset, external standard should be added with really
Recognize cutting edge of a knife or a sword position.Exceed the scope of inspection line as detected signal, then must dilute determinand solution and reanalyse；Every five kinds of differences
Sample must do the most several groups of data of duplicate detection to guarantee the repeatability of accuracy and sample.
Detection limit (limit of detection, LOD) computing formula:
D=3N/S (1)
In formula: N noise；S detector sensitivity；D detects limit；
The computing formula of sensitivity is:
S=I/Q (2)
In formula: S detector sensitivity；I signal response value；Q sample size；
Formula (1) and formula (2) are merged, obtain following formula:
D=3N × Q/I (3)
In formula: Q sample size；N noise；I signal response value；
The signal to noise ratio (S/N) that I/N is under this sample size, collection of illustrative plates can be automatically analyzed by this signal to noise ratio by work station
Obtaining, general chromatograph or mass spectrum work station all can carry out Analysis SNR calculating.
One, the scope of application:
This method is be applicable to analyzing 19 kinds of chlorophenol compositions dyestuff substrate.If desired for higher chromatography resolution or
The resistivity water sample to be measured (ultra-pure water) more than 18M Ω * cm, or carry out one or many purifying step institute with reference to this method
During the extract obtained, it is proposed that use and separate tubing string, mouth is filtered in filtration or other basic handling technique purifies.The detection of this method
The limit is the most unalterable, its result can with the difference of sample mesostroma difference.
Two, interference:
The interference of this method is originated and is summarized as three major types: the most contaminated solvent, reagent or sample treatment apparatus；2. get dirty
Current-carrying gas, part, column surface or the detector surface that the gas chromatography of dye uses；3. ambient humidity change becomes with temperature
Change.If following common laboratory working specification, and maintaining sample and operating environment management and control, can substantially avoid the dry of the first kind
Disturb.But in the middle of dye test, the interference that mainly sample substrate is brought is maximum, and the chaff interference of other by-products.
The complex sample of some compounding dyestuff need to increase other purifying step on the basis of this method and process sample, to reach true
Recognize and purity required by quantitative analysis.
Organic gas pesticide (organophosphor, organic sulfur etc.) is flowed out when using wide mouth capillary column to separate simultaneously, it is also possible to
Extraction process extracts simultaneously, becomes the chaff interference of this method.If affecting detected material sample when sample impurity excess
During product, purifying step need to be increased, organic gas pesticide and remaining interfering material of remaining non-determinand are removed.
Three, equipment:
1) glass drying oven: see the relevant specification of ultrasonic vibrating extraction, silica gel tube column purification and the carbon method of purification.
2) gaseous mass analyzer gas chromatographic analysis system must have pipe end concurrently, shunting-non-shunting injecting systems and
Other related accessories, process system including entry needle, analysis tubing string, gas, electron capture detector, record/integrator or data
System.
3) gas chromatograph injecting systems is pith, if being contaminated, having chemism or cross the syringe of high temperature
Determinand all may be caused to crack.
4) analysis condition of gas chromatograph:
1. tubing string-30m × 0.25 or the molten silicon capillary post of 0.32mm internal diameter, (pillar model is DB-inside to cover SE-54
5MS or similar tubing string), film thickness is 0.25 μm, and narrow-mouth type tubing string should be installed on the non-shunting injecting systems of shunting.(peace
Prompt human relations chromatography of gases post, Agilent J&W GC Colums) tubing string specification unrestricted each laboratory must not use other to be similar to
Tubing string, laboratory can use the capillary column that other are similar, as long as there being complete written data to prove its suitability.
2. ion source model is: meteorological mass spectrograph GCMS-QP2010 (Shimadzu, SHIMADZU)；
3. injector model: automatic sampler AOC-20its (Shimadzu, SHIMADZU)
5) analysis condition of gaseous mass analyzer
1. condition is kept a grip on:
Current-carrying gas (helium): 5.74 ± 0.5KPa；
Injection part temperature: 250 ± 50 DEG C；
Final temperature: 280 ± 50 DEG C；
Initial temperature: 80 ± 50 DEG C；
Heat up and set: 80 DEG C to 280 DEG C, with 10 ± 2 DEG C of intensifications per minute.
2. ion source condition:
Ion source temperature: 230 ± 50 DEG C；
Interface temperature: 290 ± 50 DEG C；
Solvent delay: 5 ± 1 minutes；
Ionizing energy: 70 ± 5eV.
6) result calculates
The detectable limit of detection method disclosed in the present application is 0.05ppm (mg/kg), and the qualification of detection sample is except its sharp side
The long-pending calculating with concentration, the detectable limit of determinand it is also contemplated that will refuse meter when signal ratio (signal/noise) is less than 10
Calculate.Further, if the polystream phenol of determinand goes out the skew of cutting edge of a knife or a sword position, an outer standard specimen must be added and try again detection to guarantee extraction
Accuracy.Detected value represents to 2 significant digits, and formula scales is as follows:
The test amounts of χ sample, milligrams per kilogram (mg/kg)；
A1The peak area (or peak height) of polystream phenol acetas in standard sample；
V sample liquid volume, milliliter (mL)；
The content of polystream phenol in C standard sample, milligrams per kilogram (mg/kg)；
The peak area (or peak height) of polystream phenol acetas in A sample liquids；
M final sample liquid sample size, gram (g).
Four, reagent and medicated powder
1) all test analysis processes all must use the chemical reagent of reagent level or residual level (more than 99.9wt%), and
And all reagents all meets the specification ordered by analytical reagent committee of American Chemical Society, analyze experimental water specification and test methods
(GB/T 6682-1992, neq ISO 3696:1987) does not contains organic two grades of water.
2) solvent and reagent: refering to Continuous Liquid Phase-liquid-phase extraction method, ultrasonic wave concussion extraction: normal hexane, acetone, first
Benzene, isopropanol and acetic anhydride.All solvents all should be residual level or the reagent of equal levels time, and each batch solvent all should be analyzed
Determine without non-by extraction thing, to prevent interference.
3) carbon dust that purification process uses: before use, purifies at least 1 hour with 300-400 DEG C；
4) column chromatography filler: every 0.1-10g dye sample to be measured, replaces the silica gel of deactivation with 1 ± 0.001g or uses silicon
Diatomaceous earth etc., as column chromatography filler, carry out purified treatment.
4) stock standard solutions:
1. weigh the known reference material of 0.1000 ± 0.0010g with balance, be dissolved in the mixing solvent of standard configuration, and dilute
In the volumetric flask of 100mL, to prepare the stock standard solutions of 1000 ± 0.001mg/L.Purity such as reference material >
During 99wt.%, its weight can not correct and directly calculate the concentration of stock standard solutions.
2. move to above-mentioned stock standard solutions connect lid mouth in the bottle of Teflon liner screw lid and with ParafilmTM,
With-30 DEG C of cold preservation stored protected from light；This stock standard solutions must often detect whether that cracking or volatilization situation occur, especially
Thus solution prepares standard solution, and every three months or confirmation concentration should be changed when having change in real time.
5) internal standard product:
When using disclosed method, analysis personnel must select one or more internal standard product, its sample structure
Must be similar to measured matter character, prove: these internal standard product are not by method or matrix interference and are not involved in extraction process simultaneously
Reaction.Four chlorination o-methoxyphenols (Tetrachloroguajacol, No. CAS: 2539-17-5) are as internal standard product effect
Most preferably.
Five, sample and solvent preserving type:
1) after confirming sampling container cleaning, then with mixed solvent (or fixing separate solvent) moistening.Shuttle material
It is required to be glass etc. and does not disturb the material of extract.
2) extract must cold preservation in 0-4 DEG C, replacing per week once, to guarantee extract does not have what mixed proportion mixed
Variation and cause extract poor.
3) owing to some particular dye is by the time of tide, be not easily decomposed in extraction process, sample should be placed in fixing humidity
Ambient storage is to avoid extracting difficult and unnecessary moisture content interference.
Innovative point of the present invention is: the most of concern only self safety and pay no attention to the harm of environment therefore with
Toward extraction mode with standard all using finished product as master, but the attention gradually that environmental consciousness is to initial raw material, and for the original
That expects (dyestuff) analyzes the check system that polystream phenol extraction method also neither one is clear and definite, and this method overcomes drawbacks described above, real
Show and dyestuff has been analyzed more accurately.No matter kind of dyes all can be adjusted by the method and reach requirement, and more conventional spins
Fabric is checked more preferably.
Finding in many experiments result, this access method of quenching is for chlorophenic acid, chlorophenesic acid, trichlorophenol, 2,4,6,-T response rate height
Reach more than ninety percent, further provide and take analysis for chlorophenic acid, chlorophenesic acid, accurately quenching of trichlorophenol, 2,4,6,-T in dyestuff.
Experimentation is compared conventional quenching and is taken the time more quickly, and the garbage that this access method of quenching produces is less, phase
More environmentally friendly to traditional method.
Accompanying drawing explanation
Fig. 1 is sample extraction flow chart；
Fig. 2 is that polystream phenol is schemed in gas chromatograph-mass spectrometer TIC.
Detailed description of the invention
The specific embodiment being set forth below, is that the present invention is further detailed explanation, and these embodiments are only used for
The bright purpose of the present invention, limits the scope of the comprised content of the present invention never in any form.
Embodiment
Selection sample describes
The quenching of this experiment is fetched yield and is represented sample and select based on disperse dyes, be mainly it for solvent dissolving
For difficulty and its be the most large of kind of dyes on the market.Other kinds of dyes were also tested via the method, and it is quenched and takes effect
Fruit and disperse dyes there is no the biggest difference, but other less alternatives of dye moiety impurity are ignored water and processed with purifying step also
And consideration adds suitable lysate and adjusts.
Sample describes
This experiment is combined as experiment with three kinds and considers that Background Samples, Background Samples add standard specimen and standard specimen, and often organize number
Repeat six operations according to this.General detectable substance should add a solvent sample again as polluting possible examining when measuring every time in this way
Consider.As follows:
Group 1. Background Samples: 1323 yellowish-brown (Yellow Brown AB, 2015/09/10 produces, and it is special that good fortune carrys out anthracene) (n
=6):
Dye molecule extremely content:
6Wt.%；
17Wt.%；
Dispersant NNO 77Wt.%；
Group 2. additional standard specimen concentration: 10ppm, takes 100 μ L to Background Samples (n=6)；
Group 3. standard specimen: 10ppm 0.5mL；
Date of test: 2016/01/11；
1. experiment process
1) dyestuff 0.5000 ± 0.0001g is in glass container, adds acetic anhydride (excessive) and mixes；
2) by glass container as ultrasonic vibrating machine at least 30min；
3) extract mixing (being contained within the four chlorination o-methoxyphenols of 10ppm) is added；
4) add ultra-pure water (excessive) to mix with extract；
5) 1g carbon dust mixing (part more impurity sample passes through column purification method) is added；
6) 5min is separated with the centrifugation of 3000rpm to centrifuge after mixing；
7) take supernatant and filter with filtering head (0.22 μm), i.e. completing extraction step.
2. result of the test
1) formula that this Assay recovery system calculates with standard curve obtains to add the blank group of sample deduction of standard specimen,
For guaranteeing that accuracy repeats more than six times every time, and confirmatory sample damaed cordition during each time, in terms of 3 times of signal to noise ratios,
The detection limit of this method is 0.05mg/kg.
2) every kind of chlorophenol response rate is up to 92-115%, and error amount (RSD) is all within 6%.
3) board RSD value own is shown in Table 3.
Table 1: the component data of polystream phenol:
| Component | Molecular formula | Molecular weight | Boiling point (DEG C), normal pressure |
| Chlorophenic acid | C6H5ClO | 128.56 | 175-176 |
| Chlorophenesic acid | C6H4Cl2O | 163.00 | 210 |
| Trichlorophenol, 2,4,6,-T | C6H3Cl3O | 197.44 | 246 |
| Tetrachlorophenol | C6H2Cl4O | 231.89 | 164/3.059kPa |
| Pentachlorophenol | C6HCl5O | 266.34 | 309-310 |
Polystream phenol detectable substance 1-19 kind component (the CP=chlorophenic acid of Fig. 2 gas chromatogram (TIC)；DICP=dichloro
Phenol；TCP=trichlorophenol, 2,4,6,-T；TECP=tetrachlorophenol；PCP=pentachlorophenol).
Table 2: the polystream phenol response rate and error amount form
| N=6 | Average recovery rate (%) | Standard deviation value | RSD (%) |
| Chlorophenic acid | 92.89 | 4.92 | 5.30 |
| Chlorophenesic acid | 115.40 | 4.27 | 3.70 |
| Trichlorophenol, 2,4,6,-T | 115.28 | 1.31 | 1.14 |
| Tetrachlorophenol | 117.60 | 1.24 | 1.06 |
| Pentachlorophenol | 105.97 | 3.91 | 3.69 |
Table 3: board error rate form
| Title | Retention time (minute, min) | Peak area |
| Report 1 | 3.893 | 40496 |
| Report 2 | 3.894 | 41793 |
| Report 3 | 3.898 | 39708 |
| Report 4 | 3.899 | 42094 |
| Report 5 | 3.897 | 41819 |
| Meansigma methods | 3.896 | 41182 |
| Relative standard deviation RSD (%) | 0.066 | 2.504 |
3. test is discussed
(1) the in addition identification of holdup time of measured object or peak type is confirmed: quantitative manner is then with under this determinand characteristic spike
Area and converted score on mark curve and obtain, and mutually echo with the appearance time of standard substance and make comparisons mutually and obtain.
(2) holdup time permissible range, is multiplied by 5 calculating and obtains repeatedly measuring the standard deviation of the holdup time of gained.
(3) external standard need to be added with identical pre-treatment maneuver to confirm such as the sample appearance time excessively deviation of measured object
Go out the variation of cutting edge of a knife or a sword position, when excessively deviation goes out the not calculating of cutting edge of a knife or a sword position.
(4) first confirm whether instrument is normal condition before each sample introduction, and check that consumptive material uses state unnecessary to get rid of
Test problems.
Claims (8)
1. a detection method for polystream phenol in dyestuff, the steps include: dye sample to be measured and acetic anhydride acetylation, then
Sonic oscillation mix homogeneously, then with adding the mixing solvent extraction analyte of internal standard substance, gained extractive analysis thing is through carbon dust
Doing purified treatment, through column chromatography, centrifugation, aperture, < strainer filtering of 0.22 μm, obtains clarification sample, this clarification sample the most again
Product measure the content of polystream phenol through gaseous mass analyzer.
The detection method of polystream phenol in a kind of dyestuff the most according to claim 1, it is characterised in that: from described to be measured
Dye sample extracts the step obtaining clarifying sample:
1) acetylation: dye sample to be measured is mixed with acetic anhydride, acetic anhydride and reduction group in described dye sample to be measured
Mol ratio > 1, the sample ultrasonic mixed shakes at least 30min；
2) extract: to step 1) ultrasonic complete after dye sample to be measured in add mixed solvent and carry out dissolution extraction, formed homogeneous
Sample；
Different solvents is individually added into the identical purity internal standard substance more than 99.9wt.%, remixes formation mixed solvent, internal standard
Thing is 10 ± 0.05ppm at the content of mixed solvent；
The structure of described internal standard substance is close with polystream phenol, and detection temperature range in can occur, and not with treat test sample
Product, extractant react；
3) purify: by step 2) the homogeneous sample of gained, do purified treatment through carbon dust, purify through column chromatography the most again,
The sample being purified；
4) separate: by step 3) sample that purifies of gained, at least 5min of the pelleted by centrifugation with rotating speed as 2000-3500rpm,
By aperture, < strainer filtering of 0.22 μm obtains clarification sample.
The detection method of polystream phenol in a kind of dyestuff the most according to claim 1 and 2, it is characterised in that: described treats
Surveying dye sample, the mixing solvent load used in extraction process is: every 0.5 ± 0.001mL liquid dye sample to be measured or 0.5
± 0.0001g solid dye sample to be measured uses 5 ± 0.005mL to mix solvent.
The detection method of polystream phenol in a kind of dyestuff the most according to claim 1 and 2, it is characterised in that: described is mixed
Bonding solvent is two or more combination in normal hexane, toluene, isopropanol, acetone.
The detection method of polystream phenol in a kind of dyestuff the most according to claim 2, it is characterised in that: step 2) extracted
Cheng Zhong, when described dye sample to be measured includes water miscible dispersant, the dye sample to be measured after acetylation adds
The resistivity of the 0.5mL-5mL water more than 18M Ω * cm and dye sample effect to be measured, use mixed solvent dissolution extraction the most again.
The detection method of polystream phenol in a kind of dyestuff the most according to claim 1 and 2, it is characterised in that: described is interior
Mark thing is four chlorination o-methoxyphenols.
The detection method of polystream phenol in a kind of dyestuff the most according to claim 1 and 2, it is characterised in that: described carbon
Powder, purifies at least 1h with 300-400 DEG C before use.
The detection method of polystream phenol in a kind of dyestuff the most according to claim 1 and 2, it is characterised in that: described post
The column chromatography filler used in chromatography process is silica gel or the kieselguhr replacing deactivation, and every 0.1-10g dye sample to be measured is used
1 ± 0.001g column chromatography filler.
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| CN109358121A (en) * | 2018-09-04 | 2019-02-19 | 江苏德旺化工工业有限公司 | The detection method of polystream phenol in a kind of dyestuff |
| CN115015450A (en) * | 2022-05-26 | 2022-09-06 | 贵州省烟草科学研究院 | Method for analyzing metabolites in soil through microwave derivatization-quasi-target gas chromatography-mass spectrometry |
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| CN115015450A (en) * | 2022-05-26 | 2022-09-06 | 贵州省烟草科学研究院 | Method for analyzing metabolites in soil through microwave derivatization-quasi-target gas chromatography-mass spectrometry |
| CN115015450B (en) * | 2022-05-26 | 2024-05-14 | 贵州省烟草科学研究院 | Method for analyzing metabolites in soil by microwave derivatization-quasi-target gas chromatography-mass spectrometry |
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