CN108445028A - Polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product - Google Patents
Polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product Download PDFInfo
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- CN108445028A CN108445028A CN201810222760.5A CN201810222760A CN108445028A CN 108445028 A CN108445028 A CN 108445028A CN 201810222760 A CN201810222760 A CN 201810222760A CN 108445028 A CN108445028 A CN 108445028A
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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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N2021/845—Objects on a conveyor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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Abstract
The polarized light microscopy X-ray diffraction method of asbestos in a kind of qualitative detection electronic product, it is that X-ray diffraction and polarized light microscopy are observed into the method being combined, pass through the observation of petrographic microscope, it considers the optical characteristics that sample is presented in different refractivity oil and tentatively confirms asbestos type, compared with X-ray diffraction method is used alone, so that X-ray diffraction observation shoots the arrow at the target, its result is accurate, favorable reproducibility, it can be used for precise Identification and go out in electronic product sample to be tested the micro asbestos contained, the inspection of asbestos suitable for each electronic product, asbestos harm and the trade hazard of electronic product can effectively be evaded.
Description
Technical field
The present invention relates to the identification technology fields of asbestos material, more particularly to the qualitative detection side of asbestos in electronic product
Method.
Background technology
It is generally believed that fiber is the dust of the ratio between longitudinal and transverse demeter ＞ 3: 1.Asbestos belong to threadiness, are the silicon of natural fiber
The general term of matter mineral is generally divided into chrysotile and hornblend cotton two major classes, is widely used, wherein more it is important that automobile, dragging
The manufacturing sectors such as machine drawing, chemical industry, electrical equipment.Scientific research shows that asbestos have harm, international cancer to environment, health
Disease research tissue (IARC) has announced that asbestos are A class carcinogens, many trans-corporations such as SONY, DELL, Sharp, IBM
All forbid using asbestos in its product or raw material in plain text Deng also.Method currently used for asbestos in detection product mainly has：
Phase contrast microscope method, polarized light microscopic method, scanning electron microscope analysis method, projection electron microscope analysis method, X-ray diffraction method, infrared spectrum
Method, differential thermal analysis etc., but these methods are suitable for construction material, friction material, sealing material, thermal insulation material and nonmetallic
The measurement of Determination of Asbestos in mineral.And for the micro asbestos detection in electronic product, the prior art is still not perfect.X-ray is spread out
Penetrate is to judge whether to contain certain asbestos in sample according to the intensity of the content of certain mineral and its diffraction maximum is proportional
Mineral simultaneously measure its content, since serpentine and hornblend mineral itself have two kinds of fibre structure or non-fibrous structure, there is fibre
It ties up the serpentine of structure and hornblend is just known as asbestos, therefore exclusive use X-ray diffraction method carrys out precise Identification and goes out electronic product
The micro asbestos contained in sample to be tested are extremely difficult to ideal effect, thus in view of the constituent structure of asbestos complexity, single skill
Art is difficult that the method for accurately being differentiated to it, and having arbitration power excessively relies on expensive instrument and equipment, and pervasive rate is very low.This hair
Bright polarized light microscopy-the X-ray diffraction method for proposing asbestos in a kind of qualitative detection electronic product, is by X-ray diffraction and polarisation
The method that micro- sem observation is combined, result is accurate, favorable reproducibility, and instrument universality is high, can effectively evade asbestos
Harm and trade hazard.
Invention content
For problem above of the existing technology, the present invention proposes a kind of polarisation of asbestos in qualitative detection electronic product
Micro--X-ray diffraction method, is as follows：
Step 1, processing is sampled and be ashed, is sampled on electronic product to be detected, crushes be ashed in a suitable manner
Processing, to remove organic principle, ashing temperature is more than 500 DEG C；
Step 2, sample sieves, and after the electronic product sample being ashed is cooled to room temperature in drier, is ground in agate
It grinds in alms bowl and is sieved by the metallic screen in 425 μm~500 μm of aperture；
Step 3, sampling weighs the electronic product sample 20mg after screening and is placed in 100mL tool plug triangle burnings to make sample
In bottle, 40mL water is added and shakes up, is placed on magnetic stirring apparatus and stirs, stirring while draws 20 μ L with micropipette respectively
Mixed solution drops on glass slide, and after natural drying, covered instills refractive index immersion oil in coverslip edge, makes lid glass
Piece is close to glass slide, ensures that the mineral particle on glass slide is not overlapped and is not in suspended state；
Step 4, polarized light microscopy is observed, and the sample in step 3 is placed on petrographic microscope objective table, is existed with dispersion object lens
Particle morphology is observed under single polarisation, if finding to contain fibrous particle in sample, to the fibrous particle observed in cross-polarized light
Lower confirmation angle of extinction fiber observes its direction of vibration, tentatively to confirm the type of asbestos to there is the sample of angle of extinction；If not sending out
Contain fibrous particle in existing sample, then sampled in the electronic product to be detected with certain proportion continuation, return to step 1 to
3, fibrous particle is not contained in the electronic product to be detected until confirming；
Step 5, the qualitative confirmation of the X-ray diffraction of asbestos will be uniformly filled in after step 2 treated sample
On X-ray diffraction analysis instrument sample frame, the spy that X-ray diffraction analysis condition confirmation analysis sample whether there is asbestos is further pressed
Levy diffraction maximum；If so, then containing asbestos in the electronic product to be detected；If nothing, in the electronic product to be detected
Without asbestos.
Further, in step 4 polarized light microscopy observation, various stones known to observational record under petrographic microscope in advance
The optical characteristics that cotton is presented in different refractivity oil has the direction of vibration of the sample of angle of extinction that can not but judge described in the observation
When going out possible asbestos type, step 3 is repeated, different refractivity immersion oil is added and makes more parts of samples, then carries out polarized light microscopy sight
It surveys, when the fibrous particle observed has every optical characteristics of certain asbestos recorded in advance, then preliminary identification is seen
Fiber is such asbestos, carries out step 5；Otherwise, the fibrous particle observed is not asbestos fibre particle, the electricity to be detected
Asbestos are free of in sub- product.
Further, the incineration condition for carrying out ashing processing in the step 1 to electronic product is 450 DEG C, ashing time
It is 1 hour.
Further, in the step 4 polarized light microscopy observation, particle shape is observed under single polarisation using 10 times of dispersion object lens
Looks count fibrous particle in the circle of 100 μm of diameter, and the mobile visual field, at least observe 100 particles, record sample
Middle fibrous particle number, parallel determination at least three times, if in the multiple particles for measuring observation, i.e., >=300 in particle, have
Fibrous particle then contains fibrous particle in sample.
Further, in the step 4 polarized light microscopy observation, there is the vibration of the sample of angle of extinction using 40 times of object lens observations
Direction.
Further, various asbestos known to observational record are presented in different refractivity oil under petrographic microscope in advance
Optical characteristics, the optical characteristics include ductility, birefringence, extinction, pleochroism and discrete dyeability.
Further, X-ray diffraction analysis condition described in step 5 is tube voltage 40-45kV, tube current 30-
45mA, X-ray are copper to cathode, and monochromator is Ni filters, and 2 θ of scanning range is 5~64 °.
Polarized light microscopy-X-ray diffraction method of asbestos in above-mentioned a kind of qualitative detection electronic product proposed by the present invention, be by
X-ray diffraction and polarized light microscopy observe the method being combined, and pass through the observation of petrographic microscope, it is contemplated that sample is in different refractions
The optical characteristics that is presented in rate oil simultaneously tentatively confirms asbestos type so that X-ray diffraction observation shoots the arrow at the target, and X is used alone
Ray diffraction method is compared, and result is accurate, favorable reproducibility, can be used for precise Identification go out contain in electronic product sample to be tested it is micro-
Asbestos are measured, have reached ideal effect, the inspection of asbestos suitable for each electronic product can effectively evade the asbestos of electronic product
Harm and trade hazard.
Description of the drawings
Fig. 1 is the flow diagram of qualitative checking method of the present invention.
Specific implementation mode
The present invention is further illustrated in the following with reference to the drawings and specific embodiments.
Polarized light microscopy-X-ray diffraction method of asbestos, is as follows in a kind of qualitative detection electronic product：
Step 1, processing is sampled and is ashed, sample is placed in crucible after the sample comminution of about 5g on electronic product to be measured
In, it is put into Muffle furnace, ashing temperature is more than 500 DEG C, and organics removal matter, ashing processing is specially grey at 450 DEG C ± 10 DEG C
Change 1h.
Step 2, sample sieves, and after the electronic product sample being ashed is cooled to room temperature in drier, is ground in agate
It grinds in alms bowl and is sieved by 425 μm~500 μm of aperture metallic screen.
Step 3, sampling weighs the electronic product sample 20mg after screening and is placed in 100mL tool plug triangle burnings to make sample
It in bottle, weighs and is accurate to 0.1mg, 40mL water is added and shakes up, is placed on magnetic stirring apparatus and stirs, with micro shifting while stirring
Liquid pipe draws 20 μ L mixed solutions respectively, drops on three pieces of glass slides, after natural drying, covered, in coverslip edge
Refractive index immersion oil is instilled, coverslip is made to be close to glass slide, ensures that the sample particle on glass slide is not overlapped and is not in suspension
State.
Step 4, polarized light microscopy is observed, and the sample in step 3 is placed on petrographic microscope objective table, is existed with dispersion object lens
Particle morphology is observed under single polarisation, fibrous particle pattern is observed under single polarisation with 10 times of dispersion object lens, in 100 μm of circle of diameter
It is interior that fibrous particle is counted, and the mobile visual field, 100 particles are at least observed, fibrous particle number in sample, parallel survey are recorded
Determine three times.Various species asbestos photo in the form of the sample of certain refractive index n immersion oil under certain amplification factor is made, i.e.,
Standard diagram, for being compared with the particle morphology observed, to confirm whether the particle morphology observed is asbestos fibre
The pattern of particle；If having fibrous particle in 300 particles, the fibrous particle observed is confirmed under cross-polarized light and is disappeared
Optic angle fiber observes its direction of vibration, tentatively to confirm the type of asbestos to there is the sample of angle of extinction；Wherein, with 40 times of object lens
Its direction of vibration is observed, to confirm the type of asbestos.
When thering is the direction of vibration of the sample of angle of extinction but can not judge possible asbestos type described in the observation, exist in advance
The optical characteristics that various asbestos known to observational record are presented in different refractivity oil under petrographic microscope, referring to table 1：
The optical characteristics of different asbestos fibres under 1 petrographic microscope of table
Step 3 is repeated, different refractivity immersion oil is added and makes more parts of samples, then carries out polarized light microscopy observation, when observing
Fibrous particle when there is every optical characteristics of certain asbestos recorded in advance, then tentatively assert that the fiber seen is such stone
Cotton carries out step 5；Otherwise, the fibrous particle observed is not asbestos fibre particle, and asbestos are free of in sample.Each sample
Three parts are at least observed, i.e., at least three times, every part is at least observed 100 particles, records fibrous particle number in sample, such as parallel determination
Fruit that is, >=300 in particle, there is fibrous particle in the particle for measuring observation, then contains fibrous particle in sample, carries out X
X ray diffraction detects.
Step 5, the qualitative confirmation of the X-ray diffraction of asbestos will be uniformly filled in after step 2 treated sample
On X-ray diffraction analysis instrument sample frame, the spy that X-ray diffraction analysis condition confirmation analysis sample whether there is asbestos is further pressed
Diffraction maximum is levied, is had, then contains asbestos in the electronic product to be measured, nothing is then free of asbestos in the electronic product to be measured.
It is described to press X-ray diffraction analysis condition, it whether there is the characteristic diffraction peak of asbestos for confirmation analysis sample, carry out
3 parallel laboratory tests, specific X-ray diffraction analysis condition is referring to table 2：
The qualitative analysis condition of 2 X-ray diffraction device of table
There is characteristic diffraction peak, then contains asbestos in the electronic product to be measured, no characteristic diffraction peak, then the electronic product to be measured
In be free of asbestos.
The above embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitute, combination and/or
Simplify, is regarded as equivalent substitute mode, should all be included in the protection scope of the present invention.
Claims (7)
1. polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product, which is characterized in that specific steps are such as
Under：
Step 1, processing is sampled and is ashed, is sampled on electronic product to be detected, crushes carry out ashing processing in a suitable manner,
To remove organic principle, ashing temperature is more than 500 DEG C；
Step 2, sample sieves, after the electronic product sample being ashed is cooled to room temperature in drier, in the agate mortar
It grinds and is sieved by the metallic screen in 425 μm~500 μm of aperture；
Step 3, sampling weighs the electronic product sample 20mg after screening and is placed in 100mL tool plug conical flasks to make sample,
40mL water is added to shake up, is placed on magnetic stirring apparatus and stirs, stirring while draws 20 μ L mixing with micropipette respectively
Solution drops on glass slide, and after natural drying, covered instills refractive index immersion oil in coverslip edge, keeps coverslip tight
Glass slide is pasted, ensures that the mineral particle on glass slide is not overlapped and is not in suspended state；
Step 4, polarized light microscopy is observed, and the sample in step 3 is placed on petrographic microscope objective table, with dispersion object lens single inclined
Particle morphology is observed under light, it is true under cross-polarized light to the fibrous particle observed if finding to contain fibrous particle in sample
Recognize angle of extinction fiber, to there is the sample of angle of extinction, its direction of vibration is observed, tentatively to confirm the type of asbestos；If not finding to mark
Contain fibrous particle in this, is then sampled in the electronic product to be detected with certain proportion continuation, return to step 1 to 3, directly
Fibrous particle is not contained in the electronic product to be detected to confirming；
Step 5, the qualitative confirmation of the X-ray diffraction of asbestos will be uniformly filled in X after step 2 treated sample and penetrate
On line diffraction analysis instrument sample frame, the feature that X-ray diffraction analysis condition confirmation analysis sample whether there is asbestos is further pressed
Diffraction maximum；If so, then containing asbestos in the electronic product to be detected；If nothing, in the electronic product to be detected not
Containing asbestos.
2. polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product according to claim 1,
Be characterized in that, in step 4 polarized light microscopy observation, in advance under petrographic microscope various asbestos known to observational record in difference
The optical characteristics presented in refractive index oil has the direction of vibration of the sample of angle of extinction that can not but judge described in the observation possible
When asbestos type, step 3 is repeated, different refractivity immersion oil is added and makes more parts of samples, then carries out polarized light microscopy observation, works as observation
To fibrous particle there is every optical characteristics of certain asbestos recorded in advance when, then tentatively assert that the fiber seen is such
Asbestos carry out step 5；Otherwise, the fibrous particle observed is not asbestos fibre particle, in the electronic product to be detected not
Containing asbestos.
3. polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product according to claim 2,
It is characterized in that, the incineration condition for carrying out ashing processing in the step 1 to electronic product is 450 DEG C, and ashing time is 1 hour.
4. polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product according to claim 3,
It is characterized in that, in the step 4 polarized light microscopy observation, particle morphology is observed under single polarisation using 10 times of dispersion object lens, straight
Fibrous particle is counted in the circle that 100 μm of diameter, and the mobile visual field, at least observes 100 particles, record fiber grain in sample
Subnumber, parallel determination at least three times, if in the multiple particles for measuring observation, i.e., >=300 in particle, there is fiber grain
Son then contains fibrous particle in sample.
5. polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product according to claim 4,
It is characterized in that in the step 4 polarized light microscopy observation, there is the direction of vibration of the sample of angle of extinction using 40 times of object lens observations.
6. polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product according to claim 5,
It is characterized in that, the optics that various asbestos known to observational record are presented in different refractivity oil under petrographic microscope in advance is special
Property, the optical characteristics includes ductility, birefringence, extinction, pleochroism and discrete dyeability.
7. according to polarized light microscopy-X-ray diffraction of asbestos in a kind of any qualitative detection electronic products of claim 1-6
Method, which is characterized in that X-ray diffraction analysis condition described in step 5 is tube voltage 40-45kV, tube current 30-45mA,
X-ray is copper to cathode, and monochromator is Ni filters, and 2 θ of scanning range is 5~64 °.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778467A (en) * | 2012-07-30 | 2012-11-14 | 中国检验检疫科学研究院 | Method for detecting harmful substances of asbestos |
| CN103323470A (en) * | 2013-01-13 | 2013-09-25 | 赵景红 | Toilet powder and detection method of asbestos in talcum powder |
| CN107064190A (en) * | 2016-08-26 | 2017-08-18 | 乌鲁木齐谱尼测试科技有限公司 | The improved method of asbestos component in a kind of identification medicine |
-
2018
- 2018-03-16 CN CN201810222760.5A patent/CN108445028A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778467A (en) * | 2012-07-30 | 2012-11-14 | 中国检验检疫科学研究院 | Method for detecting harmful substances of asbestos |
| CN103323470A (en) * | 2013-01-13 | 2013-09-25 | 赵景红 | Toilet powder and detection method of asbestos in talcum powder |
| CN107064190A (en) * | 2016-08-26 | 2017-08-18 | 乌鲁木齐谱尼测试科技有限公司 | The improved method of asbestos component in a kind of identification medicine |
Non-Patent Citations (3)
| Title |
|---|
| DANIEL FARCAS等: "Evaluation of fluidized bed asbestos segregator to determine erionite in soil", 《ENVIRON EARTH SCI》 * |
| 中华人民共和国国家质量监督检验检疫总局中国国家标准化管理委员会: "制品中石棉含量测定方法", 《中华人民共和国国家标准》 * |
| 高源: "建筑和汽车材料中石棉检测方法研究和风险分析", 《中国优秀硕士学位论文全文数据库》 * |
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Application publication date: 20180824 |