CN107860831A - The detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff - Google Patents
The detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff Download PDFInfo
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Abstract
The invention discloses a kind of detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in dyestuff, its step is：Sodium bicarbonate aqueous solution is added into dye sample to be measured, it is well mixed, add and mix solvent extraction analyte, mixed liquor must be extracted, extraction mixed liquor is passed through into PSA column chromatography purifications, centrifugation, filtering again, sample must be clarified, the clarification sample is through gaseous mass analyzer and using the content of the special 18 kinds of polycyclic aromatic hydrocarbons (PAH)s of post detection of Agilent chromatography of gases post, using selecting ion and external standard of arranging in pairs or groups does numerical examination.Accurate quench disclosed in the present application that take 18 kinds of polycyclic aromatic hydrocarbons (PAH) rate of recovery of method to be up to 95.44 109.37% of quenching takes analysis.And for this method no matter kind of dyes all can pass through adjustment and reach good effect of extracting, overcoming during dyestuff detects does not have the defects of detection method and standard for 18 kinds of polycyclic aromatic hydrocarbons (PAH)s.Quenched during analysis take it is more quick and and there is very good stability, and this is quenched and takes discarded object caused by method less, more environmentally friendly.
Description
Technical field
The present invention relates to a kind of detection method of harmful substance in dyestuff, and in particular in a kind of dyestuff 18 kinds it is polycyclic
The detection method of aromatic hydrocarbon.
Background technology
18 kinds of polycyclic aromatic hydrocarbons (PAH)s (Polyaromatic Hydrocarbons, PAHs) be it is a kind of containing two or two with
On phenyl ring organic compound, 18 kinds of polycyclic aromatic hydrocarbons (PAH)s are naphthalene (Naphthalene), benzo (a) pyrene (Benzo respectively
(a) pyrene), benzo (e) pyrene (Benzo (e) pyrene), 1,2 benzae thracene (Benzo (a) anthracene), 1,2- benzos
Luxuriant and rich with fragrance (Chrysene), benzo (b) fluoranthene (Benzo (b) fluoroanthene), benzo (j) fluoranthene (Benzo (j)
Fluoroanthene), benzo (k) fluoranthene (Benzo (k) fluoroanthene), dibenzanthracene (Dibenzo (a, h)
Anthracene), acenaphthene (Acenaphthene), acenaphthylene (Acenaphthylene), anthracene (Anthracene), benzo (g, h, i)
(Benzo (ghi) perylene), fluoranthene (Fluoranthene), fluorenes (Fluorene), indeno (1,2,3-cd) pyrene
(Indeno (1,2,3-cd) pyrene), luxuriant and rich with fragrance (Phenanthrene), pyrene (Pyrene).Polycyclic aromatic hydrocarbons (PAH) has carcinogenic wind more
Danger, is a fused ring compound.But international cancer research center (International Agency for Research on
Cancer, IARC) 94 kinds of compounds carcinogenic to experimental animal being listed in 1976, wherein 15 kinds are polycyclic aromatic hydrocarbon, its
In representatives of first benzo a being found as more cyclophanes, and its carcinogenicity is highest carcinogenic risk.
Polycyclic aromatic hydrocarbon is respiratory tract and skin to the main harm position of human body, if being chronically at polycyclic aromatic hydrocarbons contaminated
In environment, acute or chronic injury may be caused.Polycyclic aromatic hydrocarbon is proved animal experiment：Polycyclic aromatic hydrocarbon concentration is 0.01mg/L
There is general reaction to small white mouse, accelerating mice dying under dayligth effect, (Wang Jianqing, polycyclic aromatic hydrocarbons (PAH) is to animal and people
Carcinogenesis, modern preventive medicine 1981 (1)).
But found in plant test experiments, polycyclic aromatic hydrocarbon fall on plant leaf blade will blocking blades spiracle, make
Even come off into its discoloration, hence it is evident that influence the normal growth and result (Yue Qiang, Wang Dechao, Yu Zhiqiang, Sheng Guoying, Fu Jia of plant
Plan, 10 kinds of Hydroxyl Polycyclic Aromatics detect simultaneously in human urine, Chinese public health, 2009,25 (4):443-444).
Environmentally friendly subject under discussion is gradually concerned in recent years, is polluted increasingly caused by industrial raw material and in-between product withdraw
Seriously.Up to the present, various countries area has by what written law or decree were decided：European Union 76/769/EEC；Germany
German：GS certifications, LFGB；U.S. US：EPA；China：GB, GB/T, GHZ.According to Germany technology equipment and consumer goods committee member
The decision of meeting (ATAV), the product for carrying out GS certifications after on April 1st, 2008, it is necessary to test Environmental Protection Agency (EPA)
16 kinds of polycyclic aromatic hydrocarbons (PAH)s (PAH) of concern are to ensure compliance with related request.Environmentally friendly subject under discussion is gradually concerned in recent years, industrial
Raw material and in-between product withdraw caused by pollute getting worse, and do not have a clear and definite detection mode detection at present
The pollution rate that polycyclic aromatic hydrocarbons (PAH) uses in dyestuff, for the pollution problem of polycyclic aromatic hydrocarbons (PAH) in keyholed back plate dyestuff, need a kind of more cyclophanes
Fragrant hydrocarbon detection method ensures product quality and avoids environmental hazard to control polycyclic aromatic content.
The detection method of conventional textile has extraction power because the pure dye of characterization processes and high concentration mismatches
The problem of inadequate, furthermore the waste water that conventional detection method is discharged is more, indirectly add the burden of environment.
The content of the invention
The technical problems to be solved by the invention are：There is provided a kind of operating time it is short, extraction amount of solution it is few, waste liquid amount compared with
The detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s, the detection method can realize in dyestuff 18 kinds in low, the easy dyestuff of operation
The quick detection of polycyclic aromatic content.
In order to solve the above technical problems, the technical solution adopted in the present invention is：18 kinds of polycyclic fragrance in a kind of dyestuff
The detection method of hydrocarbon, its step are：
Sodium bicarbonate aqueous solution is added to dye sample to be measured and is well mixed, and is then added and is mixed solvent extraction analysis
Thing, gained extractive analysis thing is by PSA (solid phase is the chromatographic column of silica gel or N- propyl group ethylenediamines) column chromatography, centrifugation, filter
Net filtration, clarification sample is obtained, the clarification sample determines through gaseous mass analyzer, and uses DB-EUPAH (Agilent chromatography of gases
Post, Agilent J＆W GC Colums) special 18 kinds of polycyclic aromatic hydrocarbons (PAH)s of post detection content, using selecting ion and arrange in pairs or groups
External standard does numerical examination.This analysis method reaches mainly for 18 kinds of polycyclic aromatic hydrocarbons (PAH) detections, its sample recovery rate in dyestuff
95.44-109.37%, and the relative standard deviation (Relative Standard Deviation, RSD) of repetition detection≤
10%, respectively dyestuff mark-on, dyestuff blank and standard sample (each group sample number, N=6).
It is described to extract to obtain concretely comprising the following steps for clarification sample from dye sample to be measured：
1) being uniformly dispersed：Dye sample to be measured is mixed with 1 ± 0.5mol/L sodium bicarbonate aqueous solutions, mixed
It is 25-30 DEG C that sample keeps operating environment through ultrasonic vibration 20-30min, treats that dyestuff can be (as long as sodium bicarbonate water in even phase
Solution can blend together dyestuff even phase, and dosage is generally higher than 3ml)；
2) extract：Mixed solvent, which is added, into be measured dye sample of the ultrasound obtained by step 1) after complete carries out dissolution extraction,
It is required that dye sample to be measured is formed homogeneously with mixed solvent, to ensure that fully dissolving is (according to different dyes between dyestuff and solvent
Structure, the species of dispersant adjust to mixing time, addition lysate and sodium bicarbonate aqueous solution concentration)；
3) purify：The homogeneous sample that dye sample to be measured obtained by step 2) and mixed solvent are formed, is passed through
Cleanert PSA (Beaune Ai Jieer) column chromatography is purified, and reduces the signal strength of impact analysis thing；
Described PSA column chromatographies filler is silica gel or N- propyl group ethylenediamines, before use, first with 1 ± 0.5 ml extraction
Activated with mixed solvent, then carried out post, finally excessively complete pillar is carried out residual with 1 ± 0.5ml extraction with mixed solvent again
Stay wash-off.
4) separate：The sample that will have been purified obtained by step 3), using rotating speed as 2000-3500rpm centrifuge at least
5min, to ensure that impurity removes completely, the strainer filtering of last via hole diameter≤0.22 μm obtains defecation, and gained defecation takes
Go out, detected using the dedicated columns of gaseous mass analyzer.
Described dye sample to be measured, the mixing solvent load used in extraction process are：Every 0.5 ± 0.001mL liquid
Dye sample or 0.5 ± 0.0001g solid dye sample to be measured to be measured mixes solvent using 5 ± 0.005mL.
Described mixed solvent is that n-hexane and any of isopropanol compare mixture.
The resistivity of water used is more than 18M Ω * cm in described sodium bicarbonate aqueous solution, and described sodium acid carbonate is water-soluble
Liquid addition is added based on 0.5mL-5mL as in 0.5000 ± 0.001g dye samples to be measured.
Dye sample to be measured described in step 1) mixes with sodium bicarbonate aqueous solution, and every 0.5000 ± 0.001g is to be measured
The preferably required sodium bicarbonate aqueous solution amount of dye sample is 3ml-5ml.
Explanation:Each sample must add composition to be measured (internal standard method or external standard method) to determine the rate of recovery of the sample
And detectable limit；There is the situation of the more interference of background value to the determinand of sample, and cause the extraction of internal standard compound gurry sample
Method, it is both needed to handle in advance before analysis；, should when sample interference value is higher than the situation of measured object or causes retention time to offset
External standard is added to confirm cutting edge of a knife or a sword position.The scope that signal exceedes inspection line is such as detected, then must dilute determinand solution and again
Analysis；Repetition detection wherein several groups of data must be done in every five kinds of different samples to ensure the reappearance of accuracy and sample.
Test limit (limit of detection, LOD) calculation formula:
D=3N/S (1)
In formula：N --- noise；S --- detector sensitivity；D --- test limit；
The calculation formula of sensitivity is：
S=I/Q (2)
In formula：S --- detector sensitivity；I --- signal response；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；
I/N is the signal to noise ratio (S/N) under the sample size, and the signal to noise ratio can be divided collection of illustrative plates automatically by work station
Analysis obtains, and in general chromatogram or mass spectrum work station can all carry out Analysis signal-to-noise ratio (SNR) calculating.
First, the scope of application：
This method 18 kinds of polycyclic aromatic hydrocarbons (PAH) compositions suitable for analysis dyestuff matrix.Differentiated if desired for higher chromatography
Rate need to use the water sample to be measured (ultra-pure water) that resistivity is more than 18M Ω * cm, or one or many with reference to this method progress
During extract obtained by purifying step, it is proposed that purified using separation tubing string, filtering filter mouth or other basic handling techniques.
The detectable limit of this method is not unalterable, its result can with the difference of sample mesostroma difference.
2nd, disturb：
The interference source of this method is summarized as three major types：1. contaminated solvent, reagent or sample treatment apparatus；2. by
Current-carrying gas, part, column surface or the detector surface that the gas chromatography of pollution uses；3. ambient humidity changes and temperature
Change.If following common laboratory working specification, and sample and operating environment management and control are maintained, can substantially avoid the first kind
Interference.But among dye test, interference is maximum mainly caused by sample substrate, and the interference of other accessory substances
Thing.The complex samples of some compounding dyestuffs need to increase other purifying step processing sample on the basis of this method, with up to
Purity to required by confirmation and quantitative analysis.
The polycyclic aromatic hydrocarbons (PAH) of organic gas agricultural chemicals (organophosphor, organic sulfur etc.) or structure similar to its is using wide opening capillary
Tubing string flows out simultaneously when separating, it is also possible to is extracted simultaneously in extraction process, turns into the chaff interference of this method.If work as
Sample impurity is excessive and when influenceing detected material sample, purifying step need to be increased, by organic gas agricultural chemicals of remaining non-determinand with
And its remaining interfering material removes.
3rd, equipment：
1) glassware：Referring to ultrasonic vibrating extraction, homogeneous extraction, solid phase extraction, silicone tube column purification
Related specification.
2) gaseous mass analyzer --- gas chromatographic analysis system must have pipe end, shunting-non-shunting injecting systems concurrently
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 chemism or crossing the syringe of high temperature
May determinand be caused to crack.
4) analysis condition of gas chromatograph:
1. the capillary column (pillar model DB-EUPAH or similar tubing strings) of tubing string -20m × 0.18mm specifications, thickness
Spend for 0.14 μm, narrow-mouth type tubing string should be installed on shunting --- non-shunting injecting systems.(Agilent chromatography of gases post,
Agilent J＆W GC Colums) not other similar tubing strings, laboratory must not be used to tubing string specification by limiting each laboratory
Other similar capillary columns can be used, as long as there is complete written data to prove its applicability.
2. ion gun model:Meteorological mass spectrograph GCMS-QP2010 (Shimadzu, SHIMADZU)；
3. injector model:Automatic sampler AOC-20its (Shimadzu, SHIMADZU)
5) analysis condition of gaseous mass analyzer
1. keep a grip on condition：
Current-carrying gas (helium)：5.74±0.5KPa；
Injection part temperature：200±100℃；
Final temperature：250±100℃；
Initial temperature：80±50℃；
Heating setting：Kept for 2-4 minutes with 10 ± 5 DEG C per minute heatings；150 ± 50 DEG C of heatings are kept for 2-4 minutes；250
± 100 DEG C of holding 10-20 minutes；.
2. ion gun condition：
Ion source temperature:230±50℃；
Interface temperature:250±50℃；
Solvent delay:5 ± 2 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 identification for detecting sample removes its cutting edge of a knife or a sword
The calculating of area and concentration, the detectable limit of determinand is it is also contemplated that will not when signal ratio (signal/noise) is less than 10
Calculate.If also, when going out the skew of cutting edge of a knife or a sword position of determinand, an outer standard specimen must be added and try again detection to ensure the standard of extraction
True property.Detected value represents as follows to 2 significant digits, formula scales:
The test amounts of χ --- sample, milligrams per kilogram (mg/kg)；
A1--- the peak area (or peak height) of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in standard sample；
V --- sample liquid volume, milliliter (mL)；
C --- the content of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in standard sample, milligrams per kilogram (mg/kg)；
A --- the peak area (or peak height) of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in sample liquids；
M --- final sample fluid samples amount, gram (g).
4th, reagent and medicinal powder
1) all test analysis processes must use the chemical reagent of reagent level or residual level (more than 99.9wt%),
And all reagents meet the specification ordered by the analytical reagent committee of American Chemical Society, experimental water specification and experiment are analyzed
Method (GB/T 6682-1992, neq ISO 3696:1987) the two level water of organic matter is free of.
2) solvent and reagent：Refer to Continuous Liquid Phase-liquid-phase extraction method, ultrasonic oscillation extraction：N-hexane, isopropyl
Alcohol, sodium acid carbonate and.All solvents should be the reagent of residual level or equal level, and each batch solvent all should analyze determination
Without non-by extraction thing, to prevent from disturbing.
3) PSA (N- propyl group ethylenediamines solid-phase extraction column) that purification process uses：Need to use activating solvent before use；Often
The same product assessment of scenario of 0.1-10g, is 0.1-0.5 ± 0.001g using quantity of solvent, is substituted for the silica gel or use of deactivation
The basic cleaning of substances such as diatomite.
4) stock standard solutions：
1. weighing 0.1000 ± 0.0010g known reference material with balance, it is dissolved in the mixing solvent of standard configuration, and it is dilute
Release in 100mL volumetric flask, to prepare 1000 ± 0.001mg/L stock standard solutions.Such as the purity of reference material>
During 99wt.%, its 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 Teflon liner screw lid and connect lid with ParafilmTM
Mouthful, with -30 DEG C of refrigeration stored protected from light；This stock standard solutions must often detect whether to crack or volatilization situation, especially
It is that thus solution prepares standard liquid, and every three months or confirms that concentration has and should be changed in real time during change.
5th, sample and solvent preserving type：
1) after confirming sampling container cleaning, then with mixed solvent (or fixation separate solvent) wetting.Shuttle material
It need to be the material that glass etc. does not disturb extract.
2) extract must be refrigerated in 0-4 DEG C, per week to change once, to ensure extract does not have what mixed mixing ratio
Example variation and cause extract poor.
3) because some particular dyes are not easily decomposed by the time of tide, in extraction process, sample should be placed in fixed humidity
Ambient storage is disturbed with avoiding extracting difficult and unnecessary moisture content.
The innovative point of the application is：Environmentally friendly subject under discussion is gradually concerned in recent years, industrial raw material and in-between product
Getting worse is polluted caused by discharge, and does not have polycyclic aromatic hydrocarbons (PAH) in a clear and definite detection mode detection dyestuff to make at present
Pollution rate, for the pollution problem of polycyclic aromatic hydrocarbons (PAH) in keyholed back plate dyestuff, a kind of polycyclic aromatic hydrocarbons (PAH) detection method is needed to control
Polycyclic aromatic content processed, ensure product quality and avoid environmental hazard.
The detection method of conventional textile has extraction power because the pure dye of characterization processes and high concentration mismatches
The problem of inadequate, furthermore the waste water that conventional detection method is discharged is more, indirectly add the burden of environment.In order to make up
The deficiency of characterization processes, the more than efficiency high of this detection method can one-time detection majority sample, while detect after waste water can be weaving
Product detection mode reduces more than 50%.
Found in many experiments result, disclosed in the present application quench takes the method polycyclic aromatic hydrocarbons (PAH) rate of recovery may be up to
95.44-109.37% accurate quench takes analysis, and this method all can reach good extraction regardless of kind of dyes by adjustment
Take effect.It was found that, the rate of recovery in sample can be obviously improved through the dye sample in weak base, and we
The Agilent DB-EUPAH dedicated columns that method coordinates obtain 18 kinds of good polycyclic aromatic hydrocarbons (PAH)s of separation rate with good Parameter Conditions
Testing result, collocation selects ion and external standard of arranging in pairs or groups does numerical examination.
Brief description of the drawings
Fig. 1 is the extraction procedure figure of dye sample to be measured；
Fig. 2 is polycyclic aromatic hydrocarbons (PAH) in gaschromatographic mass spectrometry-chromatogram (TIC) polycyclic aromatic hydrocarbons (PAH) standard sample；
Fig. 3 to Fig. 7 is the standard curve I D1-ID18 of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s respectively.
Embodiment
The specific embodiment being set forth below, it is that the present invention is further detailed explanation, these embodiments are only used for
The bright purpose of the present invention, the scope of included content is not limit the invention in any way.
Embodiment
Select sample description：The quenching of this experiment, which fetches yield and represent sample, to be selected based on disperse dyes, mainly because its
Dissolving in solvent is the most difficult, and it is kind of dyes most large on the market.Other kinds of dyes are also via the method
Tested, it, which is quenched, takes effect to have no too big difference with disperse dyes, because kind of dyes and the excessively complicated alternative of structure are neglected
Slightly water process and purifying step and add appropriate lysate and adjust.
Sample describes：Experiment is combined as with three kinds consider Background Samples, Background Samples mark-on sample and standard specimen in this experiment,
And every group of data are operated with repeating six times.General detectable substance should add a standard specimen again in each measurement as dirt in this way
Dye may consider.It is as follows:
The Background Samples of group 1.:Scattered black (BLACK SRLN F15121410059-1FLET, are produced, and good fortune carrys out anthracene spy) (n
=6) (table 1)
2. group of group, 1. additional standard specimen concentration:10ppm, 100 μ L ± 1 are taken to Background Samples (n=6)；
The standard specimen of group 3.:10ppm 0.5mL±0.01；
Date of test:2016/5/20；
1. experiment process
1) for 0.5000 ± 0.001g of dyestuff into glass container, addition is more than 1 (mol/L) molar concentration
Sodium bicarbonate aqueous solution mixing 0.5-5ml；
Table 1：Dyestuff component, molecular structure and its content：
2) glass container is placed in ultrasonic vibrating machine concussion 20-30min and maintains 25-30 DEG C；
3) 5 ± 0.005ml of hybrid extraction liquid is added；
4) upper strata is taken and with 0.1-0.5g PSA (N- propyl group ethylenediamines solid-phase extraction column) column purification；
5) 5min is separated with 3000 ± 100rpm centrifugation to centrifuge after the completion of purifying；
6) take supernatant and with the filtering of (0.22 μm) of organic filter head, that is, complete extraction step.
2. result of the test
1) formula that this Assay recovery system is calculated with standard curve with add the sample of standard specimen deduct blank group and
, to ensure that the degree of accuracy repeats more than six times every time, 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 0.05mg/kg.
2) every kind of polycyclic aromatic hydrocarbons (PAH) rate of recovery is up to 95.44-109.37%, and error amount (RSD) is within 10%.
3) board RSD values ginseng itself is auspicious in table 4
Table 2：The component data of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s：
Table 3：The polycyclic aromatic hydrocarbons (PAH) rate of recovery and error amount form
Table 4：Board error rate form
| Title | Retention time (minute, min) | Peak area |
| Average value | 3.896 | 41182 |
| Relative standard deviation RSD (%) | 0.066 | 2.504 |
3. experiment discusses
(1) confirm that the holdup time of measured object or peak type are recognized：Quantitative manner is then with the determinand characteristic spike
Under area and mark song line on converted score and obtain, and mutually echoed with the appearance time of standard items and mutual make comparisons and obtain.
(2) holdup time permissible range, the standard deviation repeatedly to determine the holdup time of gained be multiplied by 5 calculating and
.
(3) as the sample appearance time excessively deviation of measured object need to add external standard with identical pre-treatment gimmick to confirm
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 sample introduction every time, and check consumptive material use state so that exclude need not
The test problems wanted.
Claims (8)
1. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff, its step are：
Sodium bicarbonate aqueous solution is added into dye sample to be measured, disperses dye sample to be measured and is well mixed, adds and mixes
Solvent extraction analyte, extraction mixed liquor is obtained, then extraction mixed liquor is passed through into PSA column chromatography purifications, centrifugation, filter screen mistake
Filter, obtains clarification sample, and the clarification sample is through gaseous mass analyzer and polycyclic using special 18 kinds of the post detection of Agilent chromatography of gases
The content of aromatic hydrocarbon, using selecting ion and external standard of arranging in pairs or groups does numerical examination.
2. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff according to claim 1, it is characterised in that：It is described
Extract to obtain concretely comprising the following steps for clarification sample from dye sample to be measured：
1) being uniformly dispersed：Dye sample to be measured is mixed with 1 ± 0.5mol/L sodium bicarbonate aqueous solutions, the sample warp mixed
Ultrasonic vibration 20-30min simultaneously keeps operating environment temperature at 25-30 DEG C, until dyestuff is in even phase；
2) extract：Add mixed solvent into be measured dye sample of the ultrasound obtained by step 1) after complete, make dye sample to be measured with
Mixed solvent is formed homogeneously, carries out dissolution extraction；
3) purify：The homogeneous sample that dye sample to be measured obtained by step 2) and mixed solvent are formed, enters through PSA column chromatographies
Row purification；
Described PSA column chromatographies then carried out post, again with extraction after excessively complete pillar using preceding needing first to be activated with the solvent of extraction
Solvent is taken to carry out residual wash-off；
4) separate：The sample that will have been purified obtained by step 3), the centrifuge at least 5min using rotating speed as 2000-3500rpm,
The strainer filtering of last via hole diameter≤0.2 μm, obtain clarifying sample.
3. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff according to claim 1 or 2, it is characterised in that：
Described dye sample to be measured, the mixing solvent load used in extraction process are：Every 0.5 ± 0.001mL liquid dyestuff to be measured
Sample or 0.5 ± 0.0001g solids dye sample to be measured mix solvent using 5 ± 0.005mL.
4. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff according to claim 1 or 2, it is characterised in that：
Described mixed solvent is that n-hexane and any of isopropanol compare mixture.
5. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff according to claim 1 or 2, it is characterised in that：
The resistivity of water used is more than 18M Ω * cm in described sodium bicarbonate aqueous solution, and described sodium bicarbonate aqueous solution addition is pressed
0.5mL-5mL meters are added in 0.5000 ± 0.001g dye samples to be measured.
6. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff according to claim 1 or 2, it is characterised in that：
Column chromatography filler in described PSA column chromatographies is silica gel or N- propyl group ethylenediamines.
7. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff according to claim 2, it is characterised in that：Step
1) dye sample to be measured described in mixes with sodium bicarbonate aqueous solution, needed for every 0.5000 ± 0.001g dye samples to be measured
Sodium bicarbonate aqueous solution amount is 3ml-5ml.
8. the detection method of 18 kinds of polycyclic aromatic hydrocarbons (PAH)s in a kind of dyestuff according to claim 2, it is characterised in that：Step
3) the PSA column chromatographies described in use front activating, and residual wash-off is carried out after use, and the amount of mixed solvent used is pressed per 0.1-
10g samples with 0.1-0.5 ± 0.001g mixed solvents wash out using residual after front activating or use.
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| CN108982710A (en) * | 2018-09-28 | 2018-12-11 | 江苏德旺化工工业有限公司 | The detection method of polycyclic aromatic hydrocarbons (PAH) in a kind of dyestuff |
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