CN102778467A - Method for detecting harmful substances of asbestos - Google Patents
Method for detecting harmful substances of asbestos Download PDFInfo
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- CN102778467A CN102778467A CN2012102689560A CN201210268956A CN102778467A CN 102778467 A CN102778467 A CN 102778467A CN 2012102689560 A CN2012102689560 A CN 2012102689560A CN 201210268956 A CN201210268956 A CN 201210268956A CN 102778467 A CN102778467 A CN 102778467A
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Abstract
The invention provides a method for detecting harmful substances of asbestos. The method includes the following steps: analyzing powder-shaped samples through X-ray diffraction (XRD) analyzing, wherein when characteristic diffraction peak of the asbestos does not exist according to the XRD analyzing, the samples contain no asbestos; and when characteristic diffraction peak exists according to the XRD analyzing, performing standard electronic module (SEM) testing and electronic data switching (EDS) testing. The asbestos is one or a plurality of chrysotile, blue amphibole asbestos, straight amphibole asbestos, magnesium iron asbestos, tremolite asbestos and actinolite asbestos. The method for detecting the harmful substances of asbestos depends on the XRD analyzing, and is aided by the SEM and EDS auxiliary testing, improves analyzing accuracy and avoids wrong judgment possibly caused by the XRD analyzing.
Description
Technical field
The invention belongs to field tests, be specially the method for utilizing objectionable impurities in X-radiation test, the scanning electron microscopy test asbestos.
Background technology
Asbestos are a kind of silicates mineral products that have high-tensile, high flexible, chemically-resistant and heat erosion, electrical isolation and have spinnability, because of its extremely fireproof property, electrical insulating property and thermal insulation, become important fire prevention, insulation and insulation material.Asbestos have 6 kinds, and chrysotile is claimed chrysotile again, and chemical formula is: Mg
3Si
2O
5(OH)
4Amphibole asbestos comprise five subspecies: blue amphibole asbesto, chemical formula is: Na
2(Mg.Fe.Al)
5Si
8O
22(OH)
2Antophyllite, chemical formula is: (Mg.Fe
2+)
7Si
8O
22(OH)
2The magnesium amosite, chemical formula is: Fe
2+.Mg)
7Si
8O
22(OH)
2Tremolite asbestos, chemical formula is: Ca
2Mg
5Si
8O
22(OH)
2And actinolite asbestos, chemical formula is: Ca
2Mg
5Si
8O
22(OH)
2
For many years observation and research show, every consumption 1t asbestos in the industry, and the 10g fibrous asbestos of will having an appointment is discharged in the environment, and every 1g asbestos contain 1,000,000 first fibers approximately, and the diameter of first fiber is generally 0.5 μ m, and length is below 5 μ m.They can suspend several weeks, several months long in big G&W, cause wide regional coverage to pollute constantly.Long-term a certain amount of fibrous asbestos of suction or first fiber can cause asbestosis, lung cancer, mesothelioma of pleura, peritoneal mesothelioma and human primary gastrointestinal cancers etc., and asbestos are a kind of verified human carcinogen's things.Therefore; The country that economy is flourishing relatively pays much attention to asbestos harm; Basically or progressively forbidden various types of asbestos, its law, rules, standard are perfect relatively with relevant policy system, and the relevant technologies means of asbestos harm prevention and control are also comparatively ripe; Developing country is also in the relevant rules policy of making great efforts to advance asbestos harm prevention and control.
If it is contain asbestos in articles for daily use, plant equipment and the raw material of industry, self-evident to user's harm.Existence that a kind of method can test asbestos objectionable impurities in the different samples is proposed whether, to the technological means of improving asbestos harm prevention and control, advance the rules policy of asbestos harm prevention and control all very important.
Summary of the invention
To the weak point of prior art, the objective of the invention is to propose a kind of detection method that detects the asbestos objectionable impurities.
The concrete technical scheme that realizes the object of the invention is:
A kind of detection method of asbestos objectionable impurities; Comprise step: powdered samples is analyzed with XRD (X-ray powder diffraction); The characteristic peak that does not occur asbestos when XRD analysis; Then judge not contain asbestos,, then carry out SEM (scanning electron microscope) test and test with EDS (power spectrum) when the characteristic peak of asbestos appears in XRD analysis.
Wherein, said asbestos are one or more in chrysotile, blue amphibole asbesto, antophyllite, magnesium amosite, tremolite asbestos, the actinolite asbestos.Different types of asbestos characteristic diffraction peak position is different, and concrete interplanar distance (d/nm), characteristic diffraction peak position (2 θ), diffracted intensity (I/CPS) are seen table 1.
Wherein, when test substance when containing organic material, test substance is crushed to below the size 3mm, at 400-480 ℃ of following ashing 1-3h, the sample after the screening ashing carries out XRD analysis to the sample after the screening then.
Wherein, when test substance is inorganic cake mass, test substance is pulverized the back screening, then the sample after the screening is carried out XRD analysis.
The characteristic diffraction peak that occurs asbestos when XRD analysis; Then carry out the SEM test; Reach 4 and above and carry out the EDS test and contain Si, Mg element simultaneously if observe length-diameter ratio greater than 3 fibrous material, then be judged as and contain asbestos, if above two conditions do not satisfy simultaneously and then judge and do not contain asbestos.That is to say, SEM test if observe length-diameter ratio greater than 3 fibrous material reach 4 and more than, then carry out the EDS test, EDS tests out and contains Si, Mg element simultaneously, then is judged as and contains asbestos, otherwise judge and do not contain asbestos; If 4 and above fibrous material are not observed in SEM test, promptly be judged as and do not contain asbestos.
Wherein, said EDS test is that length-diameter ratio is tested greater than 3 fibrous material.
Wherein, said screening is that the standard sieve with 45 μ m sieves, and gets the particle below the particle diameter 45 μ m.
Wherein, said SEM test is that powdered samples is applied to attached to perhaps sample being dripped on the conductive tape attached to sample stage with the ultrasonic dispersion of ethanol on the conductive tape of sample stage, tests after the drying.
Wherein, angle measurement scope 2 θ of said XRD analysis are 8-60 °.
Wherein, the amplification multiple of said SEM test is 500-20000 times.Amplify through SEM, sample is graininess under SEM.The particle of 1000 above samples of SEM test observation.The SEM instrument can be observed the particle about 1000 simultaneously.
Beneficial effect of the present invention is:
Can simply detect the asbestos in the materials such as commodity, organic material, insulation material, building materials fast and accurately, in case the harm that asbestos cause human body and environment;
The asbestos objectionable impurities detection method that can be used for multiple test substance that the present invention proposes not only depends on XRD analysis, and with the test that SEM and EDS assist XRD, has improved the accuracy of analyzing, the false judgment of avoiding XRD analysis to occur.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 cycle tyre sample.
Fig. 2 is the XRD figure spectrum of embodiment 2 talcum powder samples.
Fig. 3 is the XRD figure spectrum of embodiment 3 sepiolite samples.
Fig. 4 is the SEM collection of illustrative plates of embodiment 3 sepiolite samples.
Fig. 5 is the XRD figure spectrum of embodiment 4 brake block samples.
Fig. 6 is the SEM collection of illustrative plates of embodiment 4 brake block samples
Embodiment
Among the embodiment, the XRD diffractometer is Brooker D8FOCUS; The SEM ESEM is the S-4800 of Hitachi; The instrument that the EDS test is used is HORIBA 7593H.
Embodiment 1: the detection of asbestos objectionable impurities in the cycle tyre
Get 5g cycle tyre sample, it is shredded be the fragment below the 3mm, place porcelain crucible to put into 450 ℃ of muffle furnaces and keep 2h to carry out ashing.After the cooling, crossing the aperture is the standard sieve of 45 μ m, the sample after sieving is inserted in the sample cell of XRD, makes the edge maintenance level of sample and sample cell, and the XRD that packs into tests, and the scope of test angle 2 θ is: 8-60 °.From Fig. 1, can know there is not the characteristic diffraction peak of asbestos in the test result, then judge not contain asbestos in this sample.
Embodiment 2: the detection of asbestos objectionable impurities in the talcum powder
The talcum powder sample is inserted in the sample cell of XRD, made the edge maintenance level of sample and sample cell, the XRD that packs into tests, and the scope of test angle 2 θ is: 8-60 °.From Fig. 2, can know there is not the characteristic diffraction peak of asbestos in the test result, then not contain asbestos in this sample.
Embodiment 3: the detection of asbestos objectionable impurities in the sepiolite
The sepiolite sample is ground with mortar; Sample after the pulverizing is crossed the standard sieve that the aperture is 45 μ m, the sample after sieving is inserted in the sample cell of XRD, makes the edge maintenance level of sample and sample cell; The XRD that packs into tests, and the scope of test angle 2 θ is: 8-60 °.Can know that from Fig. 3 the cotton characteristic diffraction peak of blue amphibole is arranged in the test result, need carry out SEM and EDS further confirms.Sample after sieving is fixed on conductive tape on the sample stage of SEM, under SEM, observes then, enlargement factor is observed about 2000 particles for 1000 times; Observe length-diameter ratio greater than 3 fibrous material and surpass 4,, again this fibrous material is carried out the EDS test like Fig. 4; Test result such as table 2; From table 2, can know, contain Si, Mg element in this fibrous material, it is cotton then to contain blue amphibole in this sample.
Embodiment 4: the detection of asbestos objectionable impurities in the brake block
Get 5g brake block sample, it is shredded be the fragment below the 3mm, place porcelain crucible to put into 400 ℃ of muffle furnaces and keep 3h to carry out ashing.After the cooling, crossing the aperture is the standard sieve of 45 μ m, the sample after sieving is inserted in the sample cell of XRD, makes the edge maintenance level of sample and sample cell, and the XRD that packs into tests, and the scope of test angle 2 θ is: 8-60 °.Can know that from Fig. 5 the characteristic diffraction peak of chrysotile is arranged in the test result, need carry out SEM and EDS further confirms.The back sample that sieves is dripped on the conductive tape attached to sample stage with the ultrasonic dispersion of ethanol, and the observation under SEM of dry back is observed 4 above length-diameter ratios greater than 3 fibrous material; Like Fig. 6,3000 times of enlargement factors are carried out the EDS test to this fibrous material again; Test result such as table 3; From table 3, can know, contain Si, Mg element in this fibrous material, then contain chrysotile in this sample.
The intergranular distance of 6 kinds of asbestos of table 1, characteristic diffraction peak position, diffracted intensity
Table 2: sepiolite sample EDS testing result
Table 3: the EDS testing result of brake block
Above embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away from the present invention; Various modification and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (10)
1. the detection method of an asbestos objectionable impurities; Comprise step: powdered samples is analyzed with XRD,, then judged not contain asbestos when the characteristic diffraction peak of asbestos does not appear in XRD analysis; When the characteristic diffraction peak of asbestos appears in XRD analysis, then carry out the SEM test and test with EDS.
2. detection method as claimed in claim 1 is characterized in that, said asbestos are one or more in chrysotile, blue amphibole asbesto, antophyllite, magnesium amosite, tremolite asbestos, the actinolite asbestos.
3. detection method as claimed in claim 1 is characterized in that, when test substance when containing organic material; Test substance is crushed to below the size 3mm; At 400-480 ℃ of following ashing 1-3h,, then the sample after the screening is carried out XRD analysis with the screening of the sample after the ashing.
4. detection method as claimed in claim 1 is characterized in that, when test substance is inorganic cake mass, test substance is pulverized the back screening, then the sample after the screening is carried out XRD analysis.
5. detection method as claimed in claim 1; It is characterized in that; When the characteristic diffraction peak of asbestos appears in XRD analysis, then carry out the SEM test, reach 4 and above and carry out the EDS test and contain Si, Mg element simultaneously if observe length-diameter ratio greater than 3 fibrous material; Then be judged as and contain asbestos, do not contain asbestos if above two conditions do not satisfy then judgement simultaneously.
6. detection method as claimed in claim 5 is characterized in that, said EDS test is that length-diameter ratio is tested greater than 3 fibrous material.
7. like the arbitrary described detection method of claim 1-6, it is characterized in that said screening is the sample of getting below the particle diameter 45 μ m.
8. like the arbitrary described detection method of claim 1-6; It is characterized in that; Said SEM test is that sample is applied to attached to dripping on the conductive tape attached to sample stage with the ultrasonic dispersion of ethanol back on the conductive tape of sample stage or with sample, tests after the drying.
9. like the arbitrary described detection method of claim 1-6, it is characterized in that angle measurement scope 2 θ of said XRD analysis are 8-60 °, the sample that carries out XRD analysis is packed in the sample cell and is equal with the sample cell edge.
10. like the arbitrary described detection method of claim 1-6, it is characterized in that the amplification multiple of said SEM test is 500-20000 times; The particle of 1000 above samples of SEM test observation.
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| CN2012102689560A CN102778467A (en) | 2012-07-30 | 2012-07-30 | Method for detecting harmful substances of asbestos |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103076348A (en) * | 2012-12-29 | 2013-05-01 | 上海华碧检测技术有限公司 | Method for detecting content of asbestos in sample |
| 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 |
| CN108414551A (en) * | 2018-03-16 | 2018-08-17 | 中国检验检疫科学研究院 | Electron microscopic-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product |
| CN108445028A (en) * | 2018-03-16 | 2018-08-24 | 中国检验检疫科学研究院 | Polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product |
| CN109030530A (en) * | 2018-05-03 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | A kind of preparation method and measuring method of the pearlescent pigment cross-sectional sample for scanning electron microscope measurement |
| CN111812138A (en) * | 2020-06-08 | 2020-10-23 | 河北省产品质量监督检验研究院 | Method for measuring asbestos content in brake pad by scanning electron microscope-energy spectrometer |
-
2012
- 2012-07-30 CN CN2012102689560A patent/CN102778467A/en active Pending
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| 何乔桑等: "粉状化妆品中石棉的检测方法", 《化工时刊》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103076348A (en) * | 2012-12-29 | 2013-05-01 | 上海华碧检测技术有限公司 | Method for detecting content of asbestos in sample |
| 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 |
| CN108414551A (en) * | 2018-03-16 | 2018-08-17 | 中国检验检疫科学研究院 | Electron microscopic-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product |
| CN108445028A (en) * | 2018-03-16 | 2018-08-24 | 中国检验检疫科学研究院 | Polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product |
| CN109030530A (en) * | 2018-05-03 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | A kind of preparation method and measuring method of the pearlescent pigment cross-sectional sample for scanning electron microscope measurement |
| CN111812138A (en) * | 2020-06-08 | 2020-10-23 | 河北省产品质量监督检验研究院 | Method for measuring asbestos content in brake pad by scanning electron microscope-energy spectrometer |
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Application publication date: 20121114 |