CN109632584A - A kind of iconography rapid detection method of nanoparticle contained by sunscreen cosmetic - Google Patents
A kind of iconography rapid detection method of nanoparticle contained by sunscreen cosmetic Download PDFInfo
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- CN109632584A CN109632584A CN201910001383.7A CN201910001383A CN109632584A CN 109632584 A CN109632584 A CN 109632584A CN 201910001383 A CN201910001383 A CN 201910001383A CN 109632584 A CN109632584 A CN 109632584A
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- sunscreen cosmetic
- iconography
- detection method
- rapid detection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N2015/0038—Investigating nanoparticles
Abstract
The invention discloses a kind of iconography rapid detection methods of nanoparticle contained by sunscreen cosmetic, include the following steps: (1) sample preparation: sunscreen cosmetic sample to be measured is placed on specimen holder and is freezed;(2) plated film in ion sputtering device plated film: is transferred under liquid nitrogen temperature;(3) it observes: being transferred in freezing scanning electron microscope and carry out pattern test, amplification factor 1000-100k;(4) it analyzes: with X-ray energy scattering spectra, analysis of components in situ is carried out to observed solid particle.Present method avoids nanometer composition agglomeration and denaturations caused by the pretreatment, while also shortening the pre-treatment time of actual measurement sample, improve detection efficiency, are completely restored to the true form of sample to be tested, finally obtain infallible sample information.
Description
Technical field
The present invention relates to cosmetic daily chemical article detection fields, more particularly to nanoparticle contained by a kind of sunscreen cosmetic
Iconography rapid detection method.
Background technique
Nanometer technology product flourishes in recent years, produces to numerous areas such as biomedical research, electronics industry and chemical industries
Tremendous influence is given birth to.With the continuous social and economic development, people gradually promote the attention rate of beauty product, and nanometer
Technology is even more to be concerned in the application of cosmetic field.The size of nano-micron powder is extremely small and morphologically variable, and is had high
Ductility and penetration can be used as the active material with sterilization, sun-proof and other effects, but also as the load of other effective ingredients
Body provides new approach for the research and development of cosmetics.
At the same time, scholars and politicians from all over the world is but potential to nano material bring human health and environment
Harm is concerned.Although cosmetic manufacturers have repeatedly emphasized that the nanometer composition in its product will not permeate skin corium, but existing
Studies have shown that the cosmetic additive agent composition more than half may all promote the ability of skin infiltration, which means that such object
If matter sustained release, healthy cell can be caused stress to cause damage, in addition, acne on human skin, acne and wound
Mouth also provides a possibility that bigger to the infiltration of nanoparticle.
Currently, developed country pays high attention to the nanometer composition in cosmetics.European Union cosmetics instruction (EC
1223/2009) nano material being present in cosmetics is defined, and makeup of the clear stipulaties containing nanometer composition
Product declare in listing, risk assessment and the specific requirement of Product labelling (clause 12,16 and 19), and nano material is formally included in prison
Scope tube.
In China, nm cosmetic safety, product identification, listing certification and in terms of do not give still
Give necessary attention.To find out its cause, being brought greatly since cosmetic ingredient is extremely complex for the separation identification of nanometer composition
Technical difficulty, this is also the global problem in the field.Commercially available cosmetics are mostly organic and inorganic homogeneous mixture, nanometer
The extraction of composition will often undergo multistep extraction, centrifugation, washing, ashing processes.Since nanoparticle has high object
Reason, chemical activity, in the extraction process of such a complexity, it may occur that serious reunion and denaturation, final product without
Method shows that these effective ingredients are present in the time of day in product, causes subsequent qualitative and quantitative study to lack accurate
Property, corresponding risk assessment can not carry out.This present Research makes the identification technology and authentication method missing of such composition,
Corresponding mating inspection criterion and system can not be established.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of iconographies of nanoparticle contained by sunscreen cosmetic quickly to examine
Survey method, the method are based on freezing Scanning electron microscopy, sample to be studied are rapidly frozen under the conditions of liquid nitrogen,
Sample is handled in the form of perfect its prototype micro of holding of realization, then through coating technique, is carried out by electron microscope
When observing, avoid nanometer composition agglomeration and denaturation caused by the pretreatment, while also shortening the pre-treatment of actual measurement sample
Between, detection efficiency is improved, the true form of sample to be tested is completely restored to, finally obtains infallible sample information.
A kind of iconography rapid detection method of nanoparticle contained by sunscreen cosmetic, includes the following steps:
(1) sample preparation: sunscreen cosmetic sample to be measured is placed on the specimen holder of freezing scanning electron microscope, by institute
Specimen holder is stated to immerse in the freezing pond in the freezing transfer equipment full of liquid nitrogen;
(2) plated film: the specimen holder after freezing is transferred to ion by the freezing transfer equipment under liquid nitrogen temperature
Plated film is carried out in sputtering equipment;
(3) it observes: being transferred in the freezing scanning electron microscope after plated film by the freezing transfer equipment and carry out shape
Looks test, amplification factor 1000-100k;
(4) it analyzes: with X-ray energy scattering spectra, analysis of components in situ is carried out to observed solid particle.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein the plated film
Material be gold, platinum or cadmium.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein described to be measured
Sunscreen cosmetic sample morphology is liquid, paste, gel or creams shape.
Sunscreen cosmetic sample morphology to be measured is liquid, paste, gel or creams shape, the solid matter in such product
(i.e. nanometer composition) can not be observed directly using conventional sweep electron microscopy, it is necessary to by washing, filtering, sintering and etc. progress
Pre-treatment thoroughly destroys its original medium, solid matter separate and collect just can be carried out observation.Above-mentioned steps not only consume
When, energy consumption, and these solid matters can be made to have lost its original dispersity, its necessary being in the sample can not be restored
Situation.And the detection technique proposed through the invention, the whole tested from sample preparation from can be completed in 30 minutes
Process, and fully understand its original microstructure and composition.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein step (1)
In, the sunscreen cosmetic sample to be measured is equably applied on the specimen holder, keeps sample surfaces horizontal, coating layer thickness model
It encloses for 0.1-1mm, specifically depending on sample original form.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein step (1)
In, the cooling time in the freezing pond is 5-15min.
Wherein, the sample after freezing need to be shifted using the dedicated unit (freezing transfer equipment) of liquid nitrogen refrigerating, and be protected
Demonstrate,proving in sample transfer process is always freezing state;Sample is transferred to from ion sputtering instrument to scanning electron microscope, is adopted
It is operated with the specimen holder for being associated with liquid nitrogen cooling storehouse, and guarantees that transfer process guarantor is always freezing state.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein the ion
The sample bin of sputtering equipment is associated with liquid nitrogen cooling device, and control sample bin temperature is -110~-150 DEG C.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein the freezing
The sample bin of scanning electron microscope is associated with liquid nitrogen cooling device, and the temperature for controlling sample bin is -105~-120 DEG C.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein step (2)
In, the plated film with a thickness of 1-5 μm.Instrument control parameters view sample reset condition, freezing state and the nanometer of coating process
Depending on the content of particle, size.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein step (3)
In, evengranular particle is found in the scanning electron microscope visual field, is determined its basic pattern, is determined whether its particle size range is in 2
Between~100nm.
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention, wherein step (4)
In, the granular particles between 2~100nm are in if any particle size range and are existed, and composition is carried out to it with X-ray energy scattering spectra
Analysis determines its composition and content.
The iconography rapid detection method difference from prior art of nanoparticle contained by sunscreen cosmetic of the present invention exists
In:
The iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the present invention relies on emerging low temperature imaging skill
Art carries out home position observation to sample to be tested.In experimentation, sample to be studied is rapidly frozen under the conditions of liquid nitrogen first,
Its original form is kept with perfection, then sample is handled by technologies such as plated films, is observed by electron microscope.This
One treatment process of sample can avoid nanometer composition agglomeration and denaturation caused by the pretreatment with high degree, while also contract
The preparation time of short actual measurement sample, improves detection efficiency, is completely restored to the true form of nano components in the product, finally
Obtain infallible sample information.
By test it is found that method of the invention can also accurately determine the composition and content of nano particle in cosmetics,
The ICP (inductively coupled plasma body-emission spectrum) of its result and primary sample is qualitative and quantitative test result is coincide.
With reference to the accompanying drawing to the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic of the invention make into
One step explanation.
Detailed description of the invention
Fig. 1 is the SEM photograph of certain brand suncream;
Fig. 2 is the SEM photograph of certain brand sun screen;
Fig. 3 is the SEM photograph that certain brand repairs Yan Shuan.
Specific embodiment
In the present invention, freezing scanning electron microscope is Hitach S4800, and freezing and transfer equipment use Leica
EMVCT100 component.The exchange pre-vacuum chamber of the component is connected with the sem analysis instrument with pre-vacuum chamber.X-ray energy
Scattering spectra (elemental analysis) is with Horiba 1X-350 progress, and metal coating is with the completion of Leica EM SCD500 ion sputtering instrument.
Embodiment 1: the detection of nanoparticle in suncream
Appropriate suncream sample is taken to be applied in the groove of specimen holder, with a thickness of 0.1mm, so that specimen holder keeps horizontal
State is fitted into refrigerating plant and freezes 10min, and being transferred to sample bin temperature is to plate platinum film in -112 DEG C of sputters, plates membrance current
12mA, plated film time 60s, about 1.5 μm of thickness, then the scanning electricity that sample bin temperature is -106 DEG C is transferred to freezing transfer device
Pattern test is carried out in sub- microscope, amplification factor 30k carries out the test of X-ray energy scattering spectra to the nanoparticle observed.
From fig. 1, it can be seen that have acicular nanoparticles in suncream, length about 80nm, diameter about 20nm.SEM observation sees that nanoparticle does not have
There is reunion, is evenly distributed.
As a comparison, the elemental composition of the sample is tested with traditional ICP (inductively coupled plasma body-emission spectrum),
Sample is not chilled, as an aqueous solution sample introduction.As known from Table 1, the composition of nanoparticle is TiO2, X-ray quantitative detection knot
Fruit is consistent with traditional IC P result.
The analysis of components result of 1 suncream of table
Comparative experimental example 1
It takes and is applied in the groove of specimen holder with the same suncream sample of embodiment 1, with a thickness of 0.1mm, so that specimen holder
Horizontality is kept, is fitted into refrigerating plant and freezes 10min, being transferred to sample bin temperature is to carry out platinum plating in -112 DEG C of sputters
The operation of film, 1 μm of thickness.When plating membrance current greater than 20mA, deposition velocity is too fast, and particle is excessive, will lead to film thickness increase,
Influence observation;There will be reverse effects when plating membrance current less than 10mA.
Can also the preparation of sample be had an impact by adjusting plated film time.When time is shorter, the platinum ingredient of deposition is particle, meeting
Obscure with the nano components in sample;When sedimentation time is too long, thicker film can be gone into, observation is caused to be not easy to carry out.
By the importance that can be seen that the thickness of plated film in comparative experimental example.
The detection of nanoparticle in 2 sun screen of embodiment
It takes sun screen sample to be applied in the groove of specimen holder, with a thickness of 1mm, so that specimen holder keeps horizontality, is packed into
10min is freezed in refrigerating plant, being transferred to sample bin temperature with the transfer device of freezing is gold-plated film in -111 DEG C of sputters,
Plate membrance current 15mA, plated film time 50s, 1.5 μm of thickness, then being transferred to sample bin temperature with freezing transfer device is -105 DEG C
Pattern test is carried out in scanning electron microscope, amplification factor 100k carries out composition test to the nanoparticle observed.From figure
2 it is found that there is spherical nanoparticle in suncream, diameter about 10nm.As known from Table 2, the composition of nanoparticle is SiO2, EDS's
Quantitative detection result is consistent with traditional IC P result.
The analysis of components result of 2 sun screen of table
Embodiment 3 repairs the detection of Yan Shuanzhong nanoparticle
It takes and repairs face frost sample in right amount and be applied in the groove of specimen holder, thickness 0.1mm, so that specimen holder keeps horizontality,
It is fitted into refrigerating plant and freezes 10min, being transferred to sample bin temperature with the transfer device of freezing is cadmium plating in -114 DEG C of sputters
Film, plate membrance current 20mA, plated film time 60s, with a thickness of 5 μm, then with freezing transfer device be transferred to sample bin temperature be-
Pattern test is carried out in 106 DEG C of scanning electron microscope, amplification factor 30k carries out composition survey to the nanoparticle observed
Examination.As can be seen from Figure 3, there are rod-like nano particle, length about 60nm, diameter about 30nm in suncream.As known from Table 3, nanoparticle
Composition be ZnO, the quantitative detection result of EDS is consistent with traditional IC P result.
Table 3 repairs the analysis of components result of Yan Shuan
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (10)
1. a kind of iconography rapid detection method of nanoparticle contained by sunscreen cosmetic, characterized by the following steps:
(1) sample preparation: sunscreen cosmetic sample to be measured is placed on the specimen holder of freezing scanning electron microscope, by the sample
Product frame immerses in the freezing pond in the freezing transfer equipment full of liquid nitrogen;
(2) plated film: the specimen holder after freezing is transferred to ion sputtering by the freezing transfer equipment under liquid nitrogen temperature
Plated film is carried out in device;
(3) it observes: progress pattern survey in the freezing scanning electron microscope being transferred to by the freezing transfer equipment after plated film
Examination, amplification factor 1000-100k;
(4) it analyzes: with X-ray energy scattering spectra, analysis of components in situ is carried out to observed solid particle.
2. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 1, feature exist
In: the material of the plated film is gold, platinum or cadmium.
3. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 1, feature exist
In: the sunscreen cosmetic sample morphology to be measured is liquid, paste, gel or creams shape.
4. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 3, feature exist
In: in step (1), the sunscreen cosmetic sample to be measured is equably applied on the specimen holder, keeps sample surfaces horizontal,
Range of coat thicknesses is 0.1-1mm.
5. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 1, feature exist
In: in step (1), the cooling time in the freezing pond is 5-15min.
6. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 1, feature exist
In: the sample bin of the ion sputtering device is associated with liquid nitrogen cooling device, and control sample bin temperature is -110~-150 DEG C.
7. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 1, feature exist
In: it is described freezing scanning electron microscope sample bin be associated with liquid nitrogen cooling device, control sample bin temperature be -105~-
120℃。
8. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 2, feature exist
In: in step (2), the plated film with a thickness of 1-5 μm.
9. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 1, feature exist
In: in step (3), evengranular particle is found in the scanning electron microscope visual field, is determined its basic pattern, is determined its particle size range
Whether between 2~100nm.
10. the iconography rapid detection method of nanoparticle contained by sunscreen cosmetic according to claim 9, feature exist
In: in step (4), the granular particles between 2~100nm are in if any particle size range and are existed, with X-ray energy scattering spectra pair
It carries out analysis of components, determines its composition and content.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114324429A (en) * | 2021-12-10 | 2022-04-12 | 浙江大学杭州国际科创中心 | Sample freezing and transmission integrated device for scanning electron microscope |
CN116930014A (en) * | 2023-09-15 | 2023-10-24 | 中国航发北京航空材料研究院 | Detection method for nickel-based superalloy nano-phase particle size |
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CN102419277A (en) * | 2011-08-16 | 2012-04-18 | 中国检验检疫科学研究院 | Identification detection method of nano titanium dioxide in sun-screening cosmetic |
CN102589962A (en) * | 2012-01-18 | 2012-07-18 | 济南康众医药科技开发有限公司 | Method for detecting mineral fiber of montmorillonite by water enrichment method |
CN104360106A (en) * | 2014-10-21 | 2015-02-18 | 中国检验检疫科学研究院 | Freezing scanning electron microscope test method for nanoparticles in cosmetics |
CN104914021A (en) * | 2014-12-15 | 2015-09-16 | 中山大学 | Method for qualitative and quantitative analysis of titanium dioxide or/and zinc oxide nanoparticles in cosmetic |
JP6078423B2 (en) * | 2013-06-17 | 2017-02-08 | 花王株式会社 | Coating film observation method |
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2019
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102419277A (en) * | 2011-08-16 | 2012-04-18 | 中国检验检疫科学研究院 | Identification detection method of nano titanium dioxide in sun-screening cosmetic |
CN102589962A (en) * | 2012-01-18 | 2012-07-18 | 济南康众医药科技开发有限公司 | Method for detecting mineral fiber of montmorillonite by water enrichment method |
JP6078423B2 (en) * | 2013-06-17 | 2017-02-08 | 花王株式会社 | Coating film observation method |
CN104360106A (en) * | 2014-10-21 | 2015-02-18 | 中国检验检疫科学研究院 | Freezing scanning electron microscope test method for nanoparticles in cosmetics |
CN104914021A (en) * | 2014-12-15 | 2015-09-16 | 中山大学 | Method for qualitative and quantitative analysis of titanium dioxide or/and zinc oxide nanoparticles in cosmetic |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114324429A (en) * | 2021-12-10 | 2022-04-12 | 浙江大学杭州国际科创中心 | Sample freezing and transmission integrated device for scanning electron microscope |
CN116930014A (en) * | 2023-09-15 | 2023-10-24 | 中国航发北京航空材料研究院 | Detection method for nickel-based superalloy nano-phase particle size |
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