CN107543859A - The quick screening method of 4 kinds of primary aromatic diamines in a kind of toy - Google Patents
The quick screening method of 4 kinds of primary aromatic diamines in a kind of toy Download PDFInfo
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- CN107543859A CN107543859A CN201710172146.8A CN201710172146A CN107543859A CN 107543859 A CN107543859 A CN 107543859A CN 201710172146 A CN201710172146 A CN 201710172146A CN 107543859 A CN107543859 A CN 107543859A
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Abstract
The invention discloses a kind of quick screening method of 4 kinds of primary aromatic diamines in toy, comprise the following steps：Testing sample is placed in the carrier containing extractant, applies high pressure, formation electron spray, which enters in ion mobility spectrometry, carries out on-line analysis, and 4 kinds of primary aromatic diamines are 2 naphthylamines, the methylaniline of 4 chlorine 2,4 aminobphenyls and benzidine.The present invention method have the advantages that quickly, stably, cost it is low, easy to operate.
Description
Technical field
The present invention relates to a kind of detection method of chemical substance, more particularly to 4 kinds of primary aromatic diamines in a kind of toy
Quick screening method.
Background technology
China is global maximum toy manufacturing nation and exported country, and the toy in the whole world nearly 70% is made in China.However, play
Tool industry is triggered while accelerating China's economic development and providing rich and varied life to numerous children by unqualified toy
Quality safety event also often occurs.The poisonous and harmful substance added in toy product can by swallowing, licking, skin contact,
The modes such as eye contact, suction enter in children's body, grave danger children's health.
At present, the method for detecting primary aromatic diamine class compound in toy mainly has gas chromatography-mass spectrum etc., but can not be same
When meet the requirement of sensitivity, selectivity and analysis throughput, and mostly instrument is heavy, cumbersome, can not meet live quick
The needs of examination.
The content of the invention
The technical problem to be solved in the present invention is to provide it is a kind of quick, stably, cost is low, 4 kinds in toy easy to operate
The quick screening method of primary aromatic diamine.
The present invention establishes a kind of nanoliter of extraction spraying and paper spraying ionization technique coupled ion migration spectrum rapid screening not
The fast sieve technology in the scene of 4 kinds of primary aromatic diamines in type toy of the same race, one kind is provided for the detection of China's toy product quality safety
Simply, quick new method.
The quick screening method of 4 kinds of primary aromatic diamines, comprises the following steps in a kind of toy：
Testing sample is placed in the carrier containing extractant, applies 2.8kV high pressures, electron spray is formed and is moved into ion
Move in spectrum and carry out on-line analysis, 4 kinds of primary aromatic diamines be 2- naphthylamines, 4- chloro-2-methyl anilines, 4- aminobphenyls and
Benzidine.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the bar of the ion mobility spectrometry
Part is as follows：
Electron spray voltage：Positive ion mode, 2100V；
Migrate tube voltage：7700V；
Migration tube temperature：175℃；
Injector temperature：175℃；
Drift about gas velocity：1.85L/min；
Migrate spectrum width：40ms；
Data acquisition rate：200000s-1；
Bradbury-Nielsen ion gatewidths：70μs；
Bradbury-Nielsen ion gate voltages：32V；
Exhaust pump pumping speed：0.55L/min.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the testing sample is finger
Paint sample, plasticine sample, wax crayon sample, liquid toy sample or water tattoo sticker sample；The carrier is borosilicic acid
Salt capillary glass tube or 1 grade of chromatogram paper substrate；The external diameter of the borosilicate glass capillary tube is 1.5mm, internal diameter 0.86mm, is grown
For 5cm, tip is 5~10 μm, and 1 grade of chromatogram paper substrate is bottom side length 0.5cm, a height of 0.7cm, drift angle are 30 °, thickness is
0.18mm triangle paper substrate.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the finger paint sample
Directly dipped with metal microelectrode, be inserted into and be pre-charged with 20 μ L volume ratios as 100:0.5 absolute ethyl alcohol:Acetic acid extraction solvent
Borosilicate glass capillary tube in, apply 2.8kV high pressures, sample completes extraction and sophisticated at it in borosilicate glass tube
Spraying is formed, on-line analysis is carried out into ion mobility spectrometry.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the plasticine sample is first
It is put into disposable syringe or plasticine testing sample preparation facilities, it is long 1 centimetre, diameter 0.5mm from its front end extrusion
Slice simultaneously stands 1 minute in atmosphere, is then put into tweezers gripping and has drawn and injected 20 μ L volume ratios as 85:15:0.5
Absolute ethyl alcohol:Ethyl acetate:The borosilicate glass capillary tube of acetic acid extraction solvent, metal microelectrode is inserted, apply 2.8kV
High pressure, primary aromatic diamine, which is completed to extract in capillary and enters ion mobility spectrometry, carries out on-line analysis.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the wax crayon sample directly applies
Smear on 1 grade of chromatogram paper substrate, 1 grade of chromatogram paper substrate is connected to high voltage power supply by metal clip, in 1 grade of chromatographic paper
It is 70 that volume ratio is added dropwise on base:30:0.3 methanol:Isopropanol:Acetic acid extraction solvent, and add 2.8kV high pressures, testing sample exists
Extraction and migration are completed inside 1 grade of chromatographic paper primary surface and paper substrate, and enters ion mobility spectrometry and carries out on-line analysis.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the liquid toy sample is straight
Dropwise addition is connect on 1 grade of chromatogram paper substrate, 1 grade of chromatogram paper substrate is connected with metal microelectrode, on 1 grade of chromatogram paper substrate
20 μ L volume ratios are added dropwise as 90:10:0.5 absolute ethyl alcohol:Water:Acetic acid extraction solvent, and add 2.8kV high pressures, sample is in paper substrate
Extraction and migration are completed inside surface and paper substrate, and enters ion mobility spectrometry and carries out on-line analysis.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the water tattoo sticker sample
It is pasted on according to application method on 1 grade of chromatogram paper substrate, 1 grade of chromatogram paper substrate is connected with metal microelectrode, at described 1 grade
20 μ L volume ratios are added dropwise on chromatogram paper substrate as 55:45:0.5 methanol:Acetonitrile:Formic acid extraction solvent, and add 2.8kV high pressures, sample
Product enter ion mobility spectrometry and carry out on-line analysis in paper substrate surface and internal completion extraction.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the plasticine testing sample
Preparation facilities includes sample cell, push rod and diameter adjustment disk；
The sample cell be upper opening cylindrical structural, including pool wall, be connected to the pool wall bottom chassis and
Two symmetrically arranged handles being connected on the outside of the lip；Multiple circular diameters are provided with the chassis not
Same sample cell outlet；
The push rod is arranged at the upper opening of the sample cell, can freely up and down be moved in the inside of the sample cell
Dynamic, the pool wall of the outer wall of the push rod and the sample cell is in close contact；
The diameter adjustment disk includes side wall and is connected to the disk body of the sidewall bottom, the center of the disk body with it is described
Chassis is in close contact with the chassis centrally through rotation connection axis connection, the disk body and can be with the rotation connection axle
Centered on freely rotate, sample export is provided with the disk body, the diameter of the sample export goes out more than the sample cell
The diameter of mouth；
The center of the rotation connection axle to the distance between the center of circle of the sample export and the axle that is rotatablely connected
The distance between center of circle that center exports to the sample cell is equal.
The quick screening method of 4 kinds of primary aromatic diamines in toy of the present invention, wherein, the sample cell outlet is 4
Individual, diameter is respectively 0.5mm, 1.0mm, 2.0mm and 3.0mm, and the push rod is made up of duroplasts, the sample cell and described straight
Footpath adjustment disk is made up of transparent plastic；Scale is provided with the outer wall of the sample cell.
The quick screening method difference from prior art of 4 kinds of primary aromatic diamines is in toy of the present invention：
The quick screening method of 4 kinds of primary aromatic diamines is spacious using two kinds of nanoliter extraction spraying and paper spraying in toy of the present invention
Open type Ionization mode, and coupled ion migration spectrum, establish the rapid screening side of 4 kinds of primary aromatic diamines in different type toy
Method.Sample is directly splined in capillary glass tube without pre-treatment, finger paint and plasticine sample, wax crayon, water wave body patch
Paper and aqua type toy are directly splined on 1 grade of chromatographic paper, are extracted and are analyzed by adding extractant and 2.8kV high pressures
Detection, whole analysis process are completed in 10ms.The inventive method is quickly, stably, live suitable for toy product quality safety
Quick detection.
The quick screening method of 4 kinds of primary aromatic diamines in the toy of the present invention is described further below in conjunction with the accompanying drawings.
Brief description of the drawings
Fig. 1 is the ion transfer spectrogram of 4 kinds of primary aromatic diamines in the present invention；
Fig. 2 is the structural representation of plasticine testing sample preparation facilities in the present invention；
Fig. 3 is Fig. 2 upward view；
Wherein, each material numberings of Fig. 1 are consistent with table 1.
All English bilinguals occurred in accompanying drawing are as follows：
Intensity:Intensity；time:Time；ms:Millisecond.
Embodiment
First, instrument and device
P-1000 types microelectrode draws instrument, borosilicate glass capillary tube (external diameter 1.5mm, internal diameter 0.86mm, long 5cm)
(Sutter companies of the U.S.)；ESW-M15P types metal microelectrode (Warner Instruments companies of the U.S.)；GA2100 types are just
Take formula ion mobility spectrometry (Excellims companies of the U.S.)：Equipped with ion fence gate controller, air filter (sulfur acid calcium and
Molecular sieve), high-resolution Ion transfer analyzer, VisIon instrument controllings and data handling system, using it is preceding with tryptophan and
Citric acid is corrected under positive and negative ion pattern to instrument respectively；Milli-Q Superpure water machines (Millipore companies of the U.S.)；
Suction pipette head used in experiment is import (Bio-Rad company of the U.S.).
2nd, material and reagent
The standard substance of 4 kinds of primary aromatic diamines is commercially available highest purity standard sample, various primary aromatic diamine standard items
1000mg/L standard reserving solutions are configured to absolute ethyl alcohol, and being diluted to hybrid standard with absolute ethyl alcohol as needed during use works
Liquid.Tryptophan and citric acid are purchased from Sigma-Alderich companies of the U.S., using being to be configured to 10 μ g/mL with methanol to be used for instrument
Correction；Experimental water is the deionized water after Milli-Q purification filterings；1 grade of chromatographic paper (thickness 0.18mm) is purchased from the U.S.
Whatman companies, base 0.5cm, high 0.7cm triangle paper substrate are cut into during use.Finger paint, plasticine, wax crayon, water
The different types of toy sample such as tattoo sticker, bubble-water totally 30, purchased from local market, supermarket and electric business platform.
3rd, experimental procedure
1st, according to the difference of testing sample, detecting step is different, specific as follows：
Finger paint sample is directly dipped with metal microelectrode, is inserted into and is pre-charged with 20 μ L volume ratios as 100:0.5
Absolute ethyl alcohol:In the borosilicate glass capillary tube of acetic acid extraction solvent, apply 2.8kV high pressures, sample is in borosilicate glass
Extraction is completed in glass pipe and forms spraying at its tip, on-line analysis is carried out into ion mobility spectrometry.
Plasticine sample is first placed into disposable syringe cavity, and long 1 centimetre, diameter are extruded from front end of the syringe needle syringe needle
0.5mm slice simultaneously stands 1 minute in atmosphere, is then put into tweezers gripping and has drawn and injected 20 μ L volume ratios and be
85:15:0.5 absolute ethyl alcohol:Ethyl acetate:The borosilicate glass capillary tube of acetic acid extraction solvent, metal microelectrode is inserted,
Apply 2.8kV high pressures, primary aromatic diamine, which is completed to extract in capillary and enters ion mobility spectrometry, carries out on-line analysis.
Wax crayon sample is applied directly on 1 grade of chromatogram paper substrate, and 1 grade of chromatogram paper substrate is connected with metal microelectrode, in 1 grade of chromatogram
It is 70 that volume ratio is added dropwise on paper substrate:30:0.3 methanol:Isopropanol:Acetic acid extraction solvent, and add 2.8kV high pressures, testing sample
In 1 grade of chromatographic paper primary surface and internal completion extraction, and enter ion mobility spectrometry and analyze.
Liquid toy sample is directly added dropwise on 1 grade of chromatogram paper substrate, and 1 grade of chromatogram paper substrate is connected with metal microelectrode, at 1 grade
20 μ L volume ratios are added dropwise on chromatogram paper substrate as 90:10:0.5 absolute ethyl alcohol:Water:Acetic acid extraction solvent, and add 2.8kV high pressures,
Sample enters ion mobility spectrometry and analyzed in paper substrate surface and internal completion extraction.
Water tattoo sticker sample is pasted on 1 grade of chromatogram paper substrate according to application method, and it is micro- that 1 grade of chromatogram paper substrate is connected with metal
Electrode, 20 μ L volume ratios are added dropwise on 1 grade of chromatogram paper substrate as 55:45:0.5 methanol:Acetonitrile:Formic acid extraction solvent, and add
2.8kV high pressures, sample enter ion mobility spectrometry and analyzed in paper substrate surface and internal completion extraction.
2nd, Ion transfer spectral condition
Electron spray voltage：Positive ion mode, 2100V；Migrate tube voltage：7700V；Migration tube temperature：175℃；Injection port
Temperature：175℃；Drift about gas velocity：1.85L/min；Migrate spectrum width：40ms；Data acquisition rate：200000s-1；Bradbury-
Nielsen ion gatewidths：70μs；Bradbury-Nielsen ion gate voltages：32V；Exhaust pump pumping speed：0.55L/
min.The transit time and detection limit of 4 kinds of primary aromatic diamines are shown in Table 1, and ion transfer spectrogram is shown in Fig. 1.
The transit time and detection limit of 14 kinds of primary aromatic diamines of table
| Sequence number | Primary aromatic diamine | Transit time/ms | Detection limit/(mg/kg) |
| 1 | 2- naphthylamines | 7.934 | 0.5 |
| 2 | 4- chloro-2-methyl anilines | 8.350 | 2.0 |
| 3 | 4- aminobphenyls | 9.493 | 1.0 |
| 4 | Benzidine | 9.827 | 1.0 |
As shown in Figures 2 and 3, the plasticine testing sample preparation facilities used in preferred embodiment of the present invention includes sample cell
1st, push rod 2 and diameter adjustment disk 3；
Sample cell 1 is the cylindrical structural of upper opening, including pool wall 101, the chassis 102 for being connected to the bottom of pool wall 101
With two symmetrically arranged handles 103 for being connected to the top outer of pool wall 101；It is provided with chassis 102 multiple circular straight
The different sample cell outlet 104 in footpath；
Push rod 2 is arranged at the upper opening of sample cell 1, can freely up and down be moved in the inside of sample cell 1, push rod 2
The pool wall 101 of outer wall and sample cell 1 be in close contact；
Diameter adjustment disk 3 includes side wall 301 and is connected to the disk body 302 of the bottom of side wall 301, the center and bottom of disk body 302
Disk 102 connects centrally through rotation connection axle 4, and disk body 302 is in close contact with chassis 102 and can be to be rotatablely connected axle 4
Center is freely rotated, and sample export 303 is provided with disk body 302, and the diameter of sample export 303 is more than sample cell outlet 104
Diameter；
The center of axle 4 is rotatablely connected to the center of the distance between the center of circle of sample export 303 and rotation connection axle 4 to sample
The distance between the center of circle of product pond outlet 104 is equal.
Sample cell outlet 104 is 4, and diameter is respectively 0.5mm, 1.0mm, 2.0mm and 3.0mm, and push rod 2 is by duroplasts system
Into sample cell 1 and diameter adjustment disk 3 are made up of transparent plastic；Scale is provided with the outer wall of sample cell 1.
Plasticine testing sample preparation facilities application method is as follows：Take plasticine sample to be fitted into sample cell 1, load onto push rod
2, diameter adjustment disk 3 is rotated, at the sample cell outlet 104 for the diameter dimension that sample export 303 is aligned to needs, pushes down on and pushes away
Bar 2, plasticine sample is slowly extruded from sample export 303, obtain long 1 centimetre, diameter 0.5mm slice and quiet in atmosphere
Put 1 minute, be then put into tweezers gripping and drawn and injected 20 μ L volume ratios as 85:15:0.5 absolute ethyl alcohol:Acetic acid
Ethyl ester:The borosilicate glass capillary tube of acetic acid extraction solvent.
For the plasticine toy sample under conventional sense, can not direct sample carried out using capillary pipe spray ionization technique
Analysis detection.And the plasticine testing sample preparation facilities of the present invention is used conveniently and efficiently to prepare suitable for borosilicic acid
The plasticine testing sample of salt capillary glass tube, and be put into borosilicate glass capillary tube, complete subsequent analysis test.
4th, result and discussion
1st, the optimization of extractant, spray voltage and paper substrate
The polarity of extractant, performance property are to extraction and spray process important, and spray voltage is to sample ions
Change degree has material impact.Effect of extracting and protonation ability are taken into account, this experiment tests a series of solvents at the beginning of 4 kinds respectively
The ionising effect of level aromatic amine, and suitable extractant is have selected respectively for different samples.Simultaneously through investigating, at the beginning of 4 kinds
The optimal ion voltage of level aromatic amine slightly has difference, and ionizing voltage is too high or too low can all suppress different primary aromatic diamines
Response, consider the respective spray voltage and response of 4 kinds of primary aromatic diamines, determine that 2100V is optimal for this method
Spray voltage.
On this basis, the present invention investigated 1 grade of chromatographic paper, 17 grades of chromatographic papers and 31ET levels chromatographic paper to wax crayon toy,
The influence of various primary aromatic diamine extraction efficiencies in finger paint toy and water tattoo sticker type toy.Because paper substrate surface is sudden and violent
Reveal substantial amounts of hydroxyl, 4 kinds of primary aromatic diamine differing chemical properties, different paper substrates and each not phase of various primary aromatic diamine combination degrees
Together, so as to cause separation and ionising effect different, therefore, the selection to paper substrate is of crucial importance.Research shows, using 1 grade of color
Manuscript is to 4 kinds of primary aromatic diamine overall response value highests.
2nd, the optimization of injector temperature and migration tube temperature
In ion mobility spectrometry analysis detection, instrument parameter has a significant impact to the response sensitivity of determinand, at a variety of groups
When dividing sample introduction analysis simultaneously, the separating degree between each component can be improved by the setting of instrument parameter.Remove ionization voltage it
The important instrument parameter of outer injector temperature and migration tube temperature.In order to avoid ion moves caused by heat exchange or other factorses
The problem of shift time poor reproducibility, the setting of migration tube temperature and injector temperature, which should try one's best, to be consistent, therefore this experiment exists
Identical numerical value is set to investigate when optimizing this two parameters, is set series of temperature (160~200 DEG C), is compared each group
Divide the response intensity in different temperatures.Test result indicates that improving migration tube and injector temperature within the specific limits can subtract
The half-peak breadth and position excursion at small ion peak, analysis reason are as its temperature raises, and can reduce air humidity and environment temperature
Spend the interference to ion signal.But temperature is too high to cause system unstable, and thus trigger ion diffusion and collision damage
Mistake is also more serious, causes ion signal to weaken on the contrary.Through investigating, most primary aromatic diamines signal at 175 DEG C is most strong, because
This, this method finally determines that migration tube and injector temperature are concurrently set as 175 DEG C.
3rd, the optimization of drift gas velocity
Drift gas species and flow velocity can influence the resolution ratio and response intensity of quasi-molecular ions.Research work shows, using air
Each component can be preferably separated as drift gas and response intensity is high, cheap.This experiment sets a series of drift air-flows
Fast (0.50~2.00L/min) observes the separating effect and response intensity of 4 kinds of primary aromatic diamines, through investigating, 1.85L/min flow velocitys
Most preferably.
4th, method detection limit
The toy samples of 4 kinds of primary aromatic diamines is not being contained after measured as blank sample, then according to side described previously
Method carries out analysis measure, as shown in table 1 with 3 times of signal-to-noise ration estimation method detection limits, experimental result.
5th, actual sample examination
The screening method established using this experiment, to 30 different types of objects for appreciation purchased from local, supermarket and electric business platform
Tool sample carries out analysis detection, the results showed that, institute's test sample product do not detect this 4 kinds of primary aromatic diamines.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
The various modifications and improvement that case is made, it all should fall into the protection domain of claims of the present invention determination.
Claims (10)
- A kind of 1. quick screening method of 4 kinds of primary aromatic diamines in toy, it is characterised in that：Comprise the following steps：Testing sample is placed in the carrier containing extractant, applies 2.8kV high pressures, electron spray is formed and enters ion mobility spectrometry Middle carry out on-line analysis, 4 kinds of primary aromatic diamines are 2- naphthylamines, 4- chloro-2-methyl anilines, 4- aminobphenyls and biphenyl Amine.
- 2. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 1, it is characterised in that：It is described from The condition of sub- migration spectrum is as follows：Electron spray voltage：Positive ion mode, 2100V；Migrate tube voltage：7700V；Migration tube temperature：175℃；Injector temperature：175℃；Drift about gas velocity：1.85L/min；Migrate spectrum width：40ms；Data acquisition rate：200000s-1；Bradbury-Nielsen ion gatewidths：70μs；Bradbury-Nielsen ion gate voltages：32V；Exhaust pump pumping speed：0.55L/min.
- 3. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 2, it is characterised in that：It is described to treat Test sample product are finger paint sample, plasticine sample, wax crayon sample, liquid toy sample or water tattoo sticker sample；It is described Carrier is borosilicate glass capillary tube or 1 grade of chromatogram paper substrate；The external diameter of the borosilicate glass capillary tube is 1.5mm, interior Footpath is 0.86mm, a length of 5cm, and tip is 5~10 μm, and 1 grade of chromatogram paper substrate is bottom side length 0.5cm, a height of 0.7cm, drift angle The triangle paper substrate for being 0.18mm for 30 °, thickness.
- 4. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 3, it is characterised in that：The hand Point at pigment sample directly to be dipped with metal microelectrode, be inserted into and be pre-charged with 20 μ L volume ratios as 100:0.5 absolute ethyl alcohol: In the borosilicate glass capillary tube of acetic acid extraction solvent, apply 2.8kV high pressures, sample completes extraction in borosilicate glass tube Take and form spraying at its tip, on-line analysis is carried out into ion mobility spectrometry.
- 5. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 3, it is characterised in that：The rubber Skin mud sample product are first placed into disposable syringe or plasticine testing sample preparation facilities, from the disposable syringe or Extrude long 1 centimetre, diameter 0.5mm slice and in atmosphere 1 point of standing in plasticine testing sample preparation facilities front end described in person Clock, then it is put into tweezers gripping and has drawn and injected 20 μ L volume ratios as 85:15:0.5 absolute ethyl alcohol:Ethyl acetate: The borosilicate glass capillary tube of acetic acid extraction solvent, metal microelectrode is inserted, apply 2.8kV high pressures, primary aromatic diamine is in hair Complete to extract and enter ion mobility spectrometry progress on-line analysis in tubule.
- 6. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 3, it is characterised in that：The wax Sample is applied directly on 1 grade of chromatogram paper substrate, and 1 grade of chromatogram paper substrate is connected to high voltage power supply by metal clip, 20 μ L volume ratios are added dropwise on 1 grade of chromatogram paper substrate as 70:30:0.3 methanol:Isopropanol:Acetic acid extraction solvent, and add 2.8kV high pressures, testing sample is completed to extract and migrated inside 1 grade of chromatographic paper primary surface and paper substrate, and is moved into ion Move spectrum and carry out on-line analysis.
- 7. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 3, it is characterised in that：The liquid Body toys sample is directly added dropwise on 1 grade of chromatogram paper substrate, and 1 grade of chromatogram paper substrate is connected with metal microelectrode, described 1 20 μ L volume ratios are added dropwise on level chromatogram paper substrate as 90:10:0.5 absolute ethyl alcohol:Water:Acetic acid extraction solvent, and add 2.8kV high Pressure, sample are completed to extract and migrated inside paper substrate surface and paper substrate, and are entered ion mobility spectrometry and carried out on-line analysis.
- 8. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 3, it is characterised in that：The water Tattoo sticker sample is pasted on 1 grade of chromatogram paper substrate according to application method, and 1 grade of chromatogram paper substrate is connected with the micro- electricity of metal Pole, 20 μ L volume ratios are added dropwise on 1 grade of chromatogram paper substrate as 90:10:0.5 absolute ethyl alcohol:Water:Acetic acid extraction solvent, and Add 2.8kV high pressures, sample enters ion mobility spectrometry and carry out on-line analysis in paper substrate surface and internal completion extraction.
- 9. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 5, it is characterised in that：The rubber Skin mud testing sample preparation facilities includes sample cell (1), push rod (2) and diameter adjustment disk (3)；The sample cell (1) is the cylindrical structural of upper opening, including pool wall (101), is connected to the pool wall (101) bottom Chassis (102) and be connected to two symmetrically arranged handles (103) of the pool wall (101) top outer；On the chassis (102) the different sample cell outlet (104) of multiple circular diameters is provided with；The push rod (2) is arranged at the upper opening of the sample cell (1), can be above and below the inside of the sample cell (1) Move freely, the outer wall of the push rod (2) is in close contact with the pool wall (101) of the sample cell (1)；The diameter adjustment disk (3) includes side wall (301) and is connected to the disk body (302) of the side wall (301) bottom, the disk The center of body (302) is connected with the chassis (102) centrally through rotation connection axle (4), the disk body (302) and the bottom Disk (102) is in close contact and can freely rotated centered on the rotation connection axle (4), is set on the disk body (302) There is sample export (303), the diameter of the sample export (303) is more than the diameter of sample cell outlet (104)；The center of the rotation connection axle (4) to the distance between the center of circle of the sample export (303) and the rotation connection It is equal that the center of axle (4) exports the distance between the center of circle of (104) to the sample cell.
- 10. the quick screening method of 4 kinds of primary aromatic diamines in toy according to claim 9, it is characterised in that：The sample Product pond outlet (104) is 4, and diameter is respectively 0.5mm, 1.0mm, 2.0mm and 3.0mm, and the push rod (2) is by duroplasts system Into the sample cell (1) and the diameter adjustment disk (3) are made up of transparent plastic；Set on the outer wall of the sample cell (1) There is scale.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5352892A (en) * | 1992-05-29 | 1994-10-04 | Cornell Research Foundation, Inc. | Atmospheric pressure ion interface for a mass analyzer |
| CN105548332A (en) * | 2016-01-14 | 2016-05-04 | 中国检验检疫科学研究院 | Rapid detection method for forbidding sudan red dye in lipstick |
| CN105606689A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of di(2-ethylhexyl) phthalate in beverages |
| WO2016107515A1 (en) * | 2014-12-31 | 2016-07-07 | 同方威视技术股份有限公司 | Sample collection, thermal analysis, and sample injection apparatus and method, and trace detection device |
| CN105806927A (en) * | 2016-05-10 | 2016-07-27 | 中国检验检疫科学研究院 | Quick detection method for ionic migration spectrum of 3 types of bromo or chloro salicyloyl anilines in cosmetics |
| CN105842328A (en) * | 2016-03-24 | 2016-08-10 | 中国检验检疫科学研究院 | Detection method for urocanic acid and ethyl urocanate in cosmetics on the basis of ion mobility spectrometry |
| CN105866229A (en) * | 2016-03-24 | 2016-08-17 | 中国检验检疫科学研究院 | Method for rapidly detecting padimate in cosmetic based on ion mobility spectrometry |
-
2017
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5352892A (en) * | 1992-05-29 | 1994-10-04 | Cornell Research Foundation, Inc. | Atmospheric pressure ion interface for a mass analyzer |
| WO2016107515A1 (en) * | 2014-12-31 | 2016-07-07 | 同方威视技术股份有限公司 | Sample collection, thermal analysis, and sample injection apparatus and method, and trace detection device |
| CN105548332A (en) * | 2016-01-14 | 2016-05-04 | 中国检验检疫科学研究院 | Rapid detection method for forbidding sudan red dye in lipstick |
| CN105606689A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of di(2-ethylhexyl) phthalate in beverages |
| CN105842328A (en) * | 2016-03-24 | 2016-08-10 | 中国检验检疫科学研究院 | Detection method for urocanic acid and ethyl urocanate in cosmetics on the basis of ion mobility spectrometry |
| CN105866229A (en) * | 2016-03-24 | 2016-08-17 | 中国检验检疫科学研究院 | Method for rapidly detecting padimate in cosmetic based on ion mobility spectrometry |
| CN105806927A (en) * | 2016-05-10 | 2016-07-27 | 中国检验检疫科学研究院 | Quick detection method for ionic migration spectrum of 3 types of bromo or chloro salicyloyl anilines in cosmetics |
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