CN109358121A - The detection method of polystream phenol in a kind of dyestuff - Google Patents
The detection method of polystream phenol in a kind of dyestuff Download PDFInfo
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- CN109358121A CN109358121A CN201811024650.4A CN201811024650A CN109358121A CN 109358121 A CN109358121 A CN 109358121A CN 201811024650 A CN201811024650 A CN 201811024650A CN 109358121 A CN109358121 A CN 109358121A
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a kind of detection methods of polystream phenol in dyestuff, comprising the following steps: firstly, by dye sample to be measured by with obtain liquid phase after acetic anhydride hybrid reaction；Then after mixed solvent formation homogeneous phase solution is added, sample internal standard compound is added；Then extracting and demixing is carried out by the way that aqueous sodium persulfate solution is added, the extraction upper liquid of acquisition detects chlorobenzene phenol content by gaseous mass analyzer after being centrifuged, being separated by filtration.Detection method of the invention can overcome chlorophenesic acid, trichlorophenol, 2,4,6,-T chromatogram integral even to cause to sentence the puzzlement that figure is quantitatively judged by accident in peak.
Description
Technical field
The invention belongs to the detection methods of polystream phenol in technical field of analytical chemistry more particularly to dyestuff.
Background technique
Pentachlorophenol (referred to as: PCP), appearance are white flakes or crystalline solid, often contain a molecular crystalline water, slightly it is hot have it is extremely strong
Pungent stink, pentachlorophenol are preservatives common in the products such as textile, leather, timber, and when burning can be changed into dioxin
Class extremely toxic substance.It animal experiment proves that PCP is the extremely toxic substance of biological carcinogenicity, and can accumulate in organism, cause not
Reversible influence.
Tetrachlorophenol on insecticide using relatively broad, also have in international cancer research institution (IARC) proposition its to biology
Influence, though the influence of human body not can not be ignored yet really.And in 2016, global environmentally protective tissue Oeko
TexStandard100 has also increased containing for previous ignored chlorophenic acid and chlorophenesic acid newly in the keyholed back plate regulations of nuisance
Amount limitation.
Previous environmental protection specification limit is confined in finished product mostly, therefore current detection method also only terminates in textile (XP-
G08015) with the standard assays of leather (ISO17070).Also, about chlorophenic acid, chlorophenesic acid in leather and textile
It yet there are no Deng 9 kinds of isomers and tetrachlorophenol with measurement while pentachlorophenol and issue relevant criterion method.Ring in recent years
Protect subject under discussion be gradually concerned, not only terminate in finished product, the nuisance ingredient of raw material also starts to focus on, the People's Republic of China (PRC) in
The detection national standard promulgated also is only restricted in the detection (GB/T24166- of tetrachlorophenol and pentachlorophenol in dyestuff within 2009
2009)。
Currently used detection method has: ISO 17070:2006 " pentachlorophenol detection method of content in leather "；National standard
GB/T 18414.2-2006 " measurement of textile chlorinated phenol "；Standard GB/T/T24166-2009 " chlorophenol in dyestuff
Measurement "；However above-mentioned detection method, have the following disadvantages: 1. current technology integrates Lian Fengzao to polystream phenol chromatogram
It is quantitatively judged by accident at figure is sentenced；2. extraction dyestuff impurity is difficult to remove in a conventional method；3. existing dyestuff extracting process stability is not high
And solvent is incomplete to dyestuff problems of dissolution.
Summary of the invention
The present invention is in view of the deficiencies of the prior art, more in the low dyestuff of waste liquid amount the present invention provides a kind of extraction solution amount is few
The detection method of chlorophenol, which can overcome chlorophenesic acid, trichlorophenol, 2,4,6,-T chromatogram integral, and even to cause to sentence figure fixed at peak
Measure the puzzlement of erroneous judgement.
For the technical purpose more than realizing, the present invention will take technical solution below: the detection of polystream phenol in a kind of dyestuff
Method, comprising the following steps:
Firstly, by dye sample to be measured by with obtain liquid phase after acetic anhydride hybrid reaction；Then mixed solvent is added to be formed
After phase solution, sample internal standard compound is added；Then extracting and demixing, the extraction upper liquid of acquisition are carried out by the way that aqueous sodium persulfate solution is added
Chlorobenzene phenol content is detected by gaseous mass analyzer after being centrifuged, being separated by filtration.
Further, specific step is as follows for the detection method of polystream phenol in dyestuff:
(1) acetylation: dye sample to be measured is mixed with acetic anhydride, and under sonic oscillation effect, makes dyestuff sample to be measured
It restores group (chlorophenol) in product sufficiently to react and dissolve with acetic anhydride, the dyestuff residue for being not involved in reaction is located at liquid phase bottom
Layer；The sample mixed passes through sonic oscillation 30min or more；
(2) it extracts: the liquid phase that extraction step (1) obtains, and mixed solvent is added and is sufficiently mixed, sample internal standard compound shape is then added
At homogeneous sample solution；The structure of the sample internal standard compound is close with polystream phenol, and can occur in detection temperature range,
And not with sample to be tested, the loss and interference for taking solvent reaction to influence extraction process of quenching；It is required that dye sample to be measured and mixed
Bonding solvent is formed homogeneously, to ensure that sufficiently dissolution is (according to different dyes structure, the type of dispersing agent to mixed between dyestuff and solvent
It adjusts with time, addition lysate).Wherein internal standard compound is 10 ± 0.05ppm in the content of solvent, and purity is higher than
99.9wt.%.
(3) it purifies: in the sample solution that step (2) obtains, aqueous sodium persulfate solution is added and forms extracting and demixing, extraction sample is molten
Remaining dyestuff in liquid；Purified treatment is done through aqueous sodium persulfate solution and anhydrous sodium sulfate, the signal for reducing interference analyte is strong
Degree.
(4) it separates: extracting the organic phase sample of extracting and demixing at the middle and upper levels, first pass through centrifuge centrifuge separation removal impurity, then
Clarified solution is obtained through filter screen filtration；
(5) it detects: the clarified solution that step (4) obtains is detected by gaseous mass analyzer.
Preferably, the mixed solvent be n-hexane, toluene, isopropanol, in propyl alcohol at least two mixture.
Preferably, the sample internal standard compound is four chlorination o-methoxyphenols.
Preferably, the temperature of extracting and purifying is 200~250 DEG C in step (3).
According to above technical solution, compared with the existing technology, the present invention has the advantage that the present invention is directed in dyestuff
Polystream phenol detection and its derivative, sample recovery rate reach 90-110%, and repeat to detect its relative standard deviation
(Relative Standard Deviation, RSD)≤3.0% (sample number, N=3).
Detailed description of the invention
Fig. 1 is the flow diagram of the detection method of polystream phenol in dyestuff of the present invention；
Fig. 2 is the gas chromatograph-mass spectrometer TIC figure using the detection method of polystream phenol in dyestuff of the present invention.
Specific embodiment
Attached drawing discloses the structural schematic diagram of preferred embodiment involved in the present invention without limitation；It is detailed below with reference to attached drawing
Ground illustrates technical solution of the present invention.
Illustrate: each sample must add ingredient to be measured (internal standard method or external standard method) to determine the rate of recovery and detection of the sample
The limit；There is the case where background value more interference to the determinand of sample, and causes the detection of the internal standard compound rate of recovery to limit and be lower than
The sample of 0.05ppm needs matrix purification process, but the extraction of most of environment and waste sample, is both needed to before analysis
Processing in advance；When sample interference value be higher than measured object the case where or when retention time being caused to deviate, external standard should be added to confirm
Cutting edge of a knife or a sword position out.The range that signal is more than inspection line is such as detected, then must dilute determinand solution and reanalyse；Every five kinds not same
Must be done in product repetition detection wherein several groups of data to ensure the reproducibility of accuracy and sample.
Detection limit (limit of detection, LOD) calculation formula:
D=3N/S (1)
In formula: N --- noise；S --- detector sensitivity；D --- detection limit；
The calculation formula of sensitivity are as follows:
S=I/Q (2)
In formula: S --- detector sensitivity；I --- signal response；Q --- sample volume；
Formula (1) and formula (2) are merged, following formula is obtained:
D=3N × Q/I (3)
In formula: Q --- sample volume；N --- noise；I --- signal response；
I/N is the signal-to-noise ratio (S/N) under the sample volume, which can automatically analyze map by work station
It obtains, general chromatography or mass spectrum work station can all carry out Analysis signal-to-noise ratio (SNR) calculating.
One, the scope of application:
This method 19 kinds of chlorophenol ingredients suitable for analysis dyestuff matrix.Such as need higher chromatography resolution ratio or
When carrying out the resulting extract liquor of one or many purifying steps with reference to this method, it is proposed that using separation tubing string, filtering filter mouth or
Other basic handling techniques are purified.The detectable limit of this method is not unalterable, and result can be with sample mesostroma
Different and difference.
Two, it interferes:
The interference source of this method is summarized as three categories: 1. contaminated solvent, reagent or sample treatment apparatus；2. contaminated
Current-carrying gas, part, column surface or the detector surface that gas chromatography uses；3. ambient humidity variation and temperature change.If
Common laboratory working specification is followed, and sample and operating environment is maintained to manage, can substantially avoid the interference of the first kind.However
In dye test, mainly interference brought by sample substrate is maximum and other by-products chaff interferent.Certain compoundings
The more complicated sample of dyestuff need to increase other purifying step processing sample on the basis of this method, to reach confirmation and quantify
The required purity of analysis.
Organic gas pesticide (organic phosphorus, organic sulfur etc.) is flowed out simultaneously when being separated using wide opening capillary column, it is also possible to extract
It extracts simultaneously in the process, becomes the chaff interferent of this method.If influence detected material sample when sample impurity is excessive,
Purifying step need to be increased, organic gas pesticide of remaining non-determinand and remaining interfering substance are removed.
Three, equipment:
1) glassware: referring to ultrasonic vibrating extraction, silicone tube column purification specification related to the carbon method of purification.
2) gaseous mass analyzer --- gas chromatographic analysis system must have both pipe end, shunt-non-shunt injecting systems and other
Related accessories, including injection needle, analysis tubing string, gas, electron capture detector, record/integrator or data processing system.
3) gas chromatograph injecting systems are pith, if being contaminated, having chemical activity or crossing the syringe of high temperature
Determinand can be caused to crack.
4) analysis condition of gas chromatograph:
1. the molten silicon capillary column of tubing string -30m × 0.25 or 0.32mm internal diameter, inside cover SE-54 (column model be DB-5MS or
Similar tubing string), film thickness is 0.25 μm, and narrow-mouth type tubing string should be installed on shunting --- non-shunt injecting systems.(Agilent gas
As chromatographic column, Agilent J&W GC Colums) not other similar pipe must not be used to tubing string specification by limiting each laboratory
Other similar capillary column can be used in column, laboratory, as long as there is complete written data to prove its applicability.
2. ion source model are as follows: meteorological mass spectrograph GCMS-QP2010 (Shimadzu, SHIMADZU)；
3. sample injector model: autosampler AOC-20its (Shimadzu, SHIMADZU)
5) analysis condition of gaseous mass analyzer
1. tubing string condition:
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；
Heating setting: it 80 DEG C to 280 DEG C, is heated up with 10 ± 2 DEG C 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 0.5ppm (mg/kg), the identification of test sample except its sharp side product with
The calculating of concentration, the detectable limit of determinand when signal ratio (signal/noise) is lower than 10 it is also contemplated that will not calculate.And
And if an outer standard specimen must be added and try again detection to ensure the standard extracted when the polystream phenol of determinand goes out cutting edge of a knife or a sword positional shift
True property.Detected value indicates that 2 significant digits, formula scales are as follows:
The test amounts of χ --- sample, milligrams per kilogram (mg/kg)；
A1 --- the peak area (or peak height) of polystream phenol acetic acid esters in standard sample；
V --- sample liquid volume, milliliter (mL)；
C --- the content of polystream phenol in standard sample, milligrams per kilogram (mg/kg)；
A --- the peak area (or peak height) of polystream phenol acetic acid esters in sample liquids；
M --- final sample fluid samples amount, gram (g).
Four, reagent and medicinal powder
1) all test analysis processes must use the chemical reagent of reagent grade or residual grade (99.9wt% or more), and institute
There is reagent to meet specification ordered by the analytical reagent committee of American Chemical Society, analyzes experimental water specification and test methods (GB/
T 6682-1992, neq ISO 3696:1987) the second level water without organic matter.
2) solvent and reagent: refering to Continuous Liquid Phase-liquid-phase extraction method, ultrasonic oscillation extraction: mixed solvent and acetic anhydride.
All solvents should be the reagent of residual grade or equal level, and each batch solvent, which should all be analyzed, to be determined without non-by extraction object, with
It prevents from interfering.
3) anhydrous sodium sulfate that purification process uses: before use, being purified at least 1 hour with 200 DEG C or more；
4) stock standard solutions:
1. weighing the known reference substance of 0.1000 ± 0.0010g with balance, it is dissolved in standard configuration solvent, and dilute
In the volumetric flask of 100mL, to prepare the stock standard solutions of 1000 ± 0.001mg/L.As reference material purity >
When 99wt.%, weight can not correct and directly calculate the concentration of stock standard solutions.
2. above-mentioned stock standard solutions are moved in the bottle of tetrafluoroethene liner screw lid and connect lid mouth with ParafilmTM,
With -30 DEG C of refrigeration stored protected from light；This stock standard solutions must often detect whether cracking or volatilization situation, especially
Thus solution prepares standard solution, and every three months or confirmation concentration have and should replace in real time when change.
5) internal standard product:
When using disclosed method, analysis personnel must select one or more internal standard product, and sample structure is necessary
Similar to measured matter property, prove simultaneously: the internal standard product are not by method or matrix interference and are not involved in extraction process reaction.
Four chlorination o-methoxyphenols (Tetrachloroguajacol, No. CAS: 2539-17-5) are best as internal standard product effect.
Five, sample and solvent preserving type:
1) after the cleaning of confirmation sampling container, then with wet with solvent.Sample container material need to not interfere the material of extract for glass etc.
Material.
3) it is not easily decomposed due to certain particular dyes by the time of tide, in extraction process, sample should be placed in fixed humidity environment
Storage is to avoid extraction difficulty and the interference of unnecessary moisture content.
Innovative point of the present invention is: the previous only safety of itself concerned by people is simultaneously paid no attention to the harm of environment therefore is extracted in the past
Take mode and standard all using finished product as master, however gradually attention of the environmental consciousness to starting raw material, and for raw material (dye
Material) an analysis polystream phenol extracting process specific check system not yet, this method overcomes drawbacks described above, realizes pair
Dyestuff is more accurately analyzed.Reach requirement regardless of dyes can all be adjusted by the method, more previous weaving product examine
It tests more preferably.
It is found in many experiments result, this extracting process rate of recovery is up to ninety percent or more, further provides for dyestuff
Accurate extractive analysis.
Experimentation compares previous quenching and takes the time more quick, and the waste for taking method to generate of quenching is less, opposite to pass
The method of system is more environmentally friendly.
The specific embodiment that face is enumerated is that the present invention is described in further detail, these embodiments are merely to illustrate this hair
Bright purpose does not limit the invention in any way the range of included content.
Embodiment
Select sample description
The recovery of extraction of this experiment represents sample selection based on disperse dyes, is mainly that it is the most tired for the dissolution of solvent
It is difficult and it is the most large of dyes on the market.Other kinds of dyes were also tested via the method, effect of extracting with
Disperse dyes have no too big difference, but the less addition lysate appropriate that can optionally consider of other dye moiety impurity is adjusted
It is whole.
Sample description
Be combined into experiment in this experiment with three kinds of groups and consider Background Samples, Background Samples mark-on sample and standard specimen, and every group of data with
It operates in triplicate.General detectable substance should add a solvent sample as the consideration of pollution possibility again in each measurement in this way.
It is as follows:
1. Background Samples of group: 1138 red (RUBINE XFTB, 2017/10/20 produces, and dragon is contained) (n=3):
Dye molecule extremely content:
The additional standard specimen concentration of group 2.: 5ppm takes 100 μ L to Background Samples (n=3)；
3. standard specimen of group: 5ppm 0.5mL；
Date of test: 2018/03/09；
1. experiment process
1) acetic anhydride (excess) mixing is added into glass container in 0.5000 ± 0.0001g of dyestuff；
2) by glass container as ultrasonic vibrating machine at least 30min；
3) extract liquor mixing is added；
4) aqueous sodium persulfate solution (excess) is added to mix with extract liquor；
5) mixing of 1g anhydrous sodium sulfate is added；
6) at least 5min is centrifugated with the speed of at least 1000rpm to centrifuge after mixing；
7) it takes supernatant and is filtered with (0.22 μm) of filtering head, is i.e. completion extraction step.
2. test result
1) this Assay recovery system is obtained with the calculated formula of standard curve with the sample deduction blank group of standard specimen is added,
More than ensuring accuracy every time in triplicate, and the confirmatory sample damaed cordition during each time, with 3 times of signal-to-noise ratio
Meter, the detection limit of this method is 0.5mg/kg.
2) every kind of chlorophenol rate of recovery is up to 90-110%, and error amount (RSD) is all within 3%.
3) board RSD value itself 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=chlorophenesic acid；
TCP=trichlorophenol, 2,4,6,-T；TECP=tetrachlorophenol；PCP=pentachlorophenol).
Table 2: the polystream phenol rate of recovery and error amount table
Table 3: board error rate table
| Title | Retention time (minute, min) | Peak area |
| Report 1 | 8.546 | 699006 |
| Report 2 | 8.545 | 698735 |
| Report 3 | 8.547 | 700933 |
| Average value | 8.546 | 699558 |
| Relative standard deviation RSD (%) | 0.012 | 0.171 |
3. test discusses
(1) confirm that the residence time of measured object or peak type are recognized: quantitative manner is then with the face under the determinand characteristic spike
Product is obtained with converted score on curve is marked, and is mutually echoed with the appearance time of standard items and mutually made comparisons and obtain.
(2) residence time permissible range, the standard deviation repeatedly to measure the resulting residence time are calculated multiplied by 5 and are obtained.
(3) as external standard need to be added with identical pre-treatment gimmick to confirm cutting edge of a knife or a sword in the sample appearance time excessively deviation of measured object
The variation of 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 sample introduction every time, and check consumptive material use state to exclude unnecessary inspection
Survey problem.Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Illustrate, it should be understood that the above is only a specific embodiment of the present invention, be not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (5)
1. the detection method of polystream phenol in a kind of dyestuff, it is characterised in that the following steps are included:
Firstly, by dye sample to be measured by with obtain liquid phase after acetic anhydride hybrid reaction；Then mixed solvent is added to be formed
After phase solution, sample internal standard compound is added；Then extracting and demixing, the extraction upper liquid of acquisition are carried out by the way that aqueous sodium persulfate solution is added
Chlorobenzene phenol content is detected by gaseous mass analyzer after being centrifuged, being separated by filtration.
2. the detection method of polystream phenol in a kind of dyestuff, comprising the following specific steps
(1) acetylation: dye sample to be measured is mixed with acetic anhydride, and under sonic oscillation effect, makes dyestuff sample to be measured
It restores group in product sufficiently to react and dissolve with acetic anhydride, the dyestuff residue for being not involved in reaction is located at liquid phase bottom；
(2) it extracts: the liquid phase that extraction step (1) obtains, and mixed solvent is added and is sufficiently mixed, sample internal standard compound shape is then added
At homogeneous sample solution；The structure of the sample internal standard compound is close with polystream phenol, and can occur in detection temperature range,
And not with sample to be tested, the loss and interference for taking solvent reaction to influence extraction process of quenching；
(3) it purifies: in the sample solution that step (2) obtains, aqueous sodium persulfate solution is added and forms extracting and demixing, extraction sample is molten
Remaining dyestuff in liquid；
(4) it separates: extracting the organic phase sample of extracting and demixing at the middle and upper levels, first pass through centrifuge centrifuge separation removal impurity, then
Clarified solution is obtained through filter screen filtration；
(5) it detects: the clarified solution that step (4) obtains is detected by gaseous mass analyzer.
3. according to claim 1 in dyestuff polystream phenol detection method, it is characterised in that: the mixed solvent is positive oneself
Alkane, toluene, isopropanol, in propyl alcohol at least two mixture.
4. according to claim 1 in dyestuff polystream phenol detection method, it is characterised in that: the sample internal standard compound be four
Chlorination o-methoxyphenol.
5. according to claim 1 in dyestuff polystream phenol detection method, it is characterised in that: extracting and purifying in step (3)
Temperature be 200~250 DEG C.
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| CN110274979A (en) * | 2019-07-26 | 2019-09-24 | 广州众力针织品有限公司 | The detection system of polystream phenol in a kind of dyestuff |
| 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 |
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| CN110274979A (en) * | 2019-07-26 | 2019-09-24 | 广州众力针织品有限公司 | The detection system of polystream phenol in a kind of dyestuff |
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| 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 |
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