CN103323470A - Toilet powder and detection method of asbestos in talcum powder - Google Patents
Toilet powder and detection method of asbestos in talcum powder Download PDFInfo
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- CN103323470A CN103323470A CN2013100107733A CN201310010773A CN103323470A CN 103323470 A CN103323470 A CN 103323470A CN 2013100107733 A CN2013100107733 A CN 2013100107733A CN 201310010773 A CN201310010773 A CN 201310010773A CN 103323470 A CN103323470 A CN 103323470A
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Abstract
The invention belongs to the field of cosmetic safety and nonmetallic mineral analysis, and discloses a toilet powder and a detection method of asbestos in talcum powder. The method comprises following steps: dispersing a small amount of the toilet powder or the talcum powder uniformly onto a specimen holder of an X-ray diffractometer; compressing the sample with a glass slide tightly; placing the sample on a sample stage of the X-ray powder diffractometer; performing preliminary screening to the asbestos in the toilet powder or the talcum powder by combination of continuous scanning and slow segmented scanning; if the result of the preliminary screening shows that the sample of the toilet powder or the talcum powder contains asbestos, placing the sample on a 200 to 400 mesh standard sieve, and gathering asbestos by sieving; gathering sample remained on the sieve as gathered sample; observing the gathered sample with an electron microscope or a polarizing microscope to detect asbestos fibers of the toilet powder or the talcum powder. The asbestos of the toilet powder or the talcum powder is detected by the method comprising three steps, wherein the three steps are: preliminary screening by the X-ray powder diffractometer, gathering by sieving, and observing by the microscope. The detection result is more accurate and reliable, and false positives are avoided. Processes of the method are simple, rapid and accurate. The method can be widely applied in detection of asbestos in baby toilet powder and talcum powder.
Description
Technical field
The present invention relates to cosmetics safety and nonmetallic mineral analysis field, specifically, is the detection conclusive evidence method of asbestos in a kind of talcum powder and the talcum powder, and relating in particular to the talcum powder is the detection conclusive evidence method of asbestos in the talcum powder of principal ingredient and the talcum powder raw material.
Background technology
Cosmetics are the compounds that directly contact with human body, and are closely bound up with human beings'health, and particularly the safety problem of skin-care products for infant is the hot issue of countries in the world common concern at present.In April, 2009, Korea S was protected in the baby powder that several famous infant article such as peaceful pharmacy and Babyra manufacturing enterprise produces, be found to contain 1 grade of carcinogen asbestos, wherein related to imported product Germany NUK baby talcum powder very famous on the Chinese market.About the cosmetics health standard, asbestos are the forbidding thing in the cosmetic material composition according to the China national Ministry of Public Health.The first two years, Chinese consumers' association finds the part medicine of Beijing and Shenzhen market sale and the sampling observation of powder class cosmetics, contains asbestos in 15.6% cosmetics and 27.8% the medicine.
Asbestos are internationally recognized one-level carcinogenic substances, and its maximum harm comes from its fiber, in case be inhaled into human body, fibrous asbestos can accumulate in the human body for many years, adhere to and are deposited on lung, may cause diseases such as lung cancer.China has clearly to provide against in cosmetics and uses this material.The asbestos that baby powder is detected are not artificial interpolations, but come from its primary raw material mineral matter--natural talcum powder, often contain the asbestos component of association in the inferior natural talcum.
Usually adopt X-ray diffractometer in conjunction with the method detection talcum powder of electron microscope or polarizing microscope and the asbestos in the talcum powder at present both at home and abroad.X-ray diffraction method is the crystal structure analysis to mineral in this method, only can detect whether to have hornblende or serpentine class mineral in the sample, can't detect hornblende or serpentine class mineral whether grow for length-diameter ratio greater than 3 fibrous asbestos.Because talcum has layer structure and under the very low situation of asbestos content, adopt the microscopic examination method very difficult to the judgement of fibrous asbestos.In view of the foregoing, need set up a kind of sensitivity, the detection method of asbestos in the talcum powder fast immediately, strengthening the safety monitoring to domestic and international skin-care products for infant, thus protection children's personal safety and health.
Summary of the invention
The objective of the invention is for improving detection accuracy and the reliability of asbestos in talcum powder and the talcum powder, at first adopt X-ray diffraction method that the asbestos in talcum powder and the talcum powder are carried out primary dcreening operation, adopt the sieve concentration method that shakes that the fibrous asbestos that contains among the primary dcreening operation result in the doubtful asbestos sample is carried out enrichment then, talcum powder and the asbestos in the talcum powder after adopting the microscopic examination method to enrichment at last carry out confirmatory analysis.
The technical scheme that the present invention adopts for achieving the above object is: the detection conclusive evidence method of asbestos in a kind of talcum powder and the talcum powder may further comprise the steps:
1, asbestos primary dcreening operation: a small amount of talcum powder or talcum powder sample are uniformly distributed on the X-ray diffraction specimen holder, be placed on the glass sheet compacting on the sample platform of powder x-ray diffraction, in conjunction with the mode of continuous sweep and fractional scanning at a slow speed the asbestos in talcum powder and the talcum powder carried out primary dcreening operation.
2, the sieve enrichment of shaking: take by weighing baby powder or talcum powder material sample 5～10g, place on 200～400 mesh standard sieves, place on the automatic pulp classifier, vibrosieve 10-15min makes granularity pass through sieve aperture fully less than the talcum powder in standard sieve aperture.Residual sample is as the enrichment sample on the collection screen.
3, microscopic examination:
(1) electron microscope observation
Sample after a small amount of enrichment is bonded on the objective table of electron microscope with conducting resinl, places under the electron microscope and observe.
(2) polarizing microscope is identified
Drip 1 at microslide and drip, a spot of enrichment sample is dispersed in the water droplet of microslide, covered is made the water logging thin slice, places under the polarizing microscope and measures.
As preferably, the X-ray diffraction specimen holder in the step 1 is glass sample frame and metallic aluminium specimen holder.
As preferably, the X-ray diffractometer condition determination in the step 1: X-ray tube is selected copper (Cu) target for use, solid probe, and pipe is pressed 40 kV; Pipe stream 40mA; Divergent slit: 1 mm; Scatter slit: 1 mm; Accept slit: 0.1 mm.
As preferably, continuous sweep condition in the step 1 is that sweep limit (2 θ) ° is 5 °～60 °, the sampling step is wide to be 0.02 °/step, sweep velocity is 4～10 °/min, the purpose of continuous sweep is to differentiate mutually for baby powder and talcous thing, to get rid of the interference that other impurity detects asbestos.
As preferably, fractional scanning condition in the step 1 is that sweep limit (2 θ) ° is 10 °～13 ° and 23 °～26 °, the sampling step is wide to be 0.02 °/step, sweep velocity is 0.1 °/min, the purpose of fractional scanning is for the discriminating of baby powder and the micro-hornblende of talcum powder and serpentine minerals at a slow speed, finishes the primary dcreening operation to asbestos.
As preferably, adopting powder X-ray diffractometry in the step 1 is in fractional scanning scope at a slow speed (2 θ: 10 °～13 ° and 23 °～26 °) to the primary dcreening operation judgment basis of asbestos, if the spectrum peak appears in the place, feature 2 θ angles at amphibole asbestos mineral, chrysotile mineral, then may contain asbestos in the preliminary judgement sample.
As preferably, it is the 200-400 order that the standard sieve in the step 2 adopts the order number, and the aperture is 75 μ m-32 μ m.
As preferably, the electron microscope enlargement factor in the step 3 from 30-1000 doubly.
As preferably, the polarizing microscope enlargement factor in the step 3 from 20-200 doubly.
As preferably, the microscopic examination method in the step 3 is length-diameter ratio greater than 3 mineral fibres to the judgment basis of asbestos.
The invention has the beneficial effects as follows: set up the powder X-ray diffractometry primary dcreening operation, shake and sieve the concentration method enrichment, the detection conclusive evidence method of asbestos in the talcum powder of microscopic examination method conclusive evidence and the talcum powder makes that the detection of asbestos is more accurate, reliable in talcum powder and the talcum powder, has avoided the false positive of detection.Experimental technique is simple, accurate, fast, can be widely used in the detection of asbestos in baby powder and the talcum powder.
Description of drawings:
Fig. 1 is the X-ray diffraction stack spectrogram that contains the talcum powder sample of asbestos mineral.
Fig. 2 is the electron micrograph (amplifying 200 times) of residual sample on talcum powder former state and 400 mesh standard sieves
Fig. 3 is the polarizing microscope photo (amplifying 100 times) of residual sample on talcum powder former state and 400 mesh standard sieves
Fig. 4 is the electron micrograph (amplifying 200 times) that contains residual sample on the talcum powder former state of fibrous asbestos and 200 mesh standard sieves
Fig. 5 is the electron micrograph (amplifying 200 times) of residual sample on the talcum powder former state of no fibrous asbestos and 200 mesh standard sieves
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail, but the present invention is not limited to specific embodiment.
The detection confirmatory analysis of asbestos in embodiment 1 talcum powder
A small amount of talcum powder sample is uniformly distributed on the X-ray diffraction specimen holder, is placed on the glass sheet compacting on the sample platform of powder x-ray diffraction, in conjunction with the mode of continuous sweep and fractional scanning at a slow speed the asbestos mineral in the talcum powder are carried out primary dcreening operation.Powder x-ray diffraction device testing conditions is: X-ray tube is selected copper (Cu) target for use, solid probe, and pipe is pressed 40 kV; Pipe stream 40mA; Divergent slit: 1 mm; Scatter slit: 1 mm; Accept slit: 0.1 mm; The purpose of continuous sweep is to differentiate mutually for talcous thing, to get rid of the interference that other impurity detects asbestos.The continuous sweep condition is that sweep limit (2 θ) ° is 5 °～60 °, and the sampling step wide is 0.02 °/step, and sweep velocity is 4-10 °/min; The purpose of fractional scanning is for the discriminating of the micro-hornblende of talcum powder and serpentine minerals at a slow speed, finishes the primary dcreening operation to asbestos.The fractional scanning condition is that sweep limit (2 θ) ° is 10 °～13 ° and 23 °～26 °, and the sampling step wide is 0.02 °/step, and sweep velocity is 0.1 °/min.
Talcum powder sample 5～10g that the primary dcreening operation result is contained doubtful asbestos mineral on 400 mesh standard sieves, with vibrosieve 10-15min on the automatic pulp classifier, make granularity less than the talcum powder in standard sieve aperture fully by sieve aperture, residual sample on the sieve.The shake method of sieve enrichment of employing is enriched in sieve with the fibrous asbestos in the talcum powder and goes up in the residual sample.
Sieve is gone up residual sample be bonded on the objective table of electron microscope with conducting resinl, place under the electron microscope and observe, regulate enlargement factor from 30 times to 1000 times, observing whether there is fibrous asbestos within sweep of the eye.
Fig. 1 is the X-ray diffraction stack spectrogram of talcum powder sample,
Fig. 2 goes up the electron micrograph of residual sample for talcum powder former state under 200 times of electron microscopes of amplification and sieve.
Fig. 3 goes up the polarizing microscope photo of residual sample for talcum powder former state under 100 times of polarizing microscopes of amplification and sieve.
As can be seen from Figure 1 detect the existence that the asbestos mineral may be arranged by powder x-ray diffraction analysis, Fig. 2 is the electron micrograph through the sample before and after the sieve concentration method enrichment of shaking, and Fig. 3 is through the polarizing microscope photo of the sample before and after the sieve concentration method enrichment of shaking.As can be seen, the fibrous asbestos in the enrichment sample is than the easier discriminating of the asbestos in the former state and conclusive evidence from Fig. 2 and Fig. 3.
The detection confirmatory analysis of asbestos in embodiment 2 baby powders
A small amount of baby powder sample is uniformly distributed on the X-ray diffraction specimen holder, is placed on the glass sheet compacting on the sample platform of powder x-ray diffraction, in conjunction with the mode of continuous sweep and fractional scanning at a slow speed the asbestos mineral in the talcum powder are carried out primary dcreening operation.Powder x-ray diffraction device testing conditions is: X-ray tube is selected copper (Cu) target for use, solid probe, and pipe is pressed 40 kV; Pipe stream 40mA; Divergent slit: 1 mm; Scatter slit: 1 mm; Accept slit: 0.1 mm; The purpose of continuous sweep is to differentiate mutually for the thing of baby powder, to get rid of the interference that other impurity detects asbestos.The continuous sweep condition is that sweep limit (2 θ) ° is 5 °～60 °, and the sampling step wide is 0.02 °/step, and sweep velocity is 4～10 °/min; The purpose of fractional scanning is for the discriminating of the micro-hornblende of baby powder and serpentine minerals at a slow speed, finishes the primary dcreening operation to asbestos.The fractional scanning condition is that sweep limit (2 θ) ° is 10 °～13 ° and 23 °～26 °, and the sampling step wide is 0.02 °/step, and sweep velocity is 0.1 °/min.
The baby powder sample 5～10g that 2 primary dcreening operation results is contained doubtful asbestos mineral is on 200 mesh standard sieves respectively, with vibrosieve 10-15min on the automatic pulp classifier, make granularity less than the talcum powder in standard sieve aperture fully by sieve aperture, residual sample on the sieve.The shake method of sieve enrichment of employing is enriched in sieve with the fibrous asbestos in the talcum powder and goes up in the residual sample.
Sieve is gone up residual sample be bonded on the objective table of electron microscope with conducting resinl, place under the electron microscope and observe, regulate enlargement factor from 30 times to 1000 times, observing whether there is fibrous asbestos within sweep of the eye.
Fig. 4 contains asbestos talcum powder former state and sieves the electron micrograph of going up residual sample for amplifying under 200 times of electron microscopes.
Fig. 5 goes up the electron micrograph of residual sample for no asbestos talcum powder former state under 200 times of electron microscopes of amplification and sieve.
To contain the talcum powder sample of asbestos by the powder x-ray diffraction primary dcreening operation, the sample through before and after the sieve concentration method enrichment of shaking detects whether contain fibrous asbestos under electron microscope.Figure 4 and 5 are the electron micrograph that 2 kinds of primary dcreening operations contain the talcum powder example enrichment front and back of asbestos, as can be seen from Figure 4, and the easier detection conclusive evidence of the fibrous asbestos in the talcum powder sample after the enrichment.As can be seen from Figure 5, for the talcum powder sample of no fibrous asbestos, there is not fibrous asbestos in the sample epigranular after the enrichment in the easier conclusive evidence sample.
Claims (10)
1. the detection conclusive evidence method of asbestos in a talcum powder and the talcum powder is characterized in that this method may further comprise the steps:
(1) asbestos primary dcreening operation: a small amount of talcum powder or talcum powder sample are uniformly distributed on the X-ray diffraction specimen holder, be placed on the glass sheet compacting on the sample platform of powder x-ray diffraction, in conjunction with the mode of continuous sweep and fractional scanning at a slow speed the asbestos in talcum powder and the talcum powder carried out primary dcreening operation;
(2) the sieve enrichment of shaking: take by weighing baby powder or talcum powder material sample 5～10g, place on 200～400 mesh standard sieves, place on the automatic pulp classifier, vibrosieve 10-15min, make granularity less than the talcum powder in standard sieve aperture fully by sieve aperture, residual sample is as the enrichment sample on the collection screen;
(3) microscopic examination:
A) electron microscope observation
Sample after a small amount of enrichment is bonded on the objective table of electron microscope with conducting resinl, places under the electron microscope and observe;
B) polarizing microscope is identified
Drip 1 at microslide and drip, a spot of enrichment sample is dispersed in the water droplet of microslide, covered is made the water logging thin slice, places under the polarizing microscope and measures.
2. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that the described X-ray diffraction specimen holder of step 1 is glass sample frame and metallic aluminium specimen holder.
3. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that the described X-ray diffractometer condition determination of step 1: X-ray tube is selected copper (Cu) target for use, solid probe, and pipe is pressed 40 kV; Pipe stream 40mA; Divergent slit: 1 mm; Scatter slit: 1 mm; Accept slit: 0.1 mm.
4. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that, the described continuous sweep condition of step 1 is that sweep limit (2 θ) ° is 5 °～60 °, the sampling step is wide to be 0.02 °/step, sweep velocity is 4～10 °/min, the purpose of continuous sweep is to differentiate mutually for baby powder and talcous thing, to get rid of the interference that other impurity detects asbestos.
5. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that, the described fractional scanning condition of step 1 is that sweep limit (2 θ) ° is 10 °～13 ° and 23 °～26 °, the sampling step is wide to be 0.02 °/step, sweep velocity is 0.1 °/min, the purpose of fractional scanning is for the discriminating of baby powder and the micro-hornblende of talcum powder and serpentine minerals at a slow speed, finishes the primary dcreening operation to asbestos.
6. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that, the described employing powder X-ray diffractometry of step 1 is in fractional scanning scope at a slow speed (2 θ: 10 °～13 ° and 23 °～26 °) to the primary dcreening operation judgment basis of asbestos, if the spectrum peak appears in the place, feature 2 θ angles at amphibole asbestos mineral, chrysotile mineral, then may contain asbestos in the preliminary judgement sample.
7. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that it is the 200-400 order that the described standard sieve of step 2 adopts the order number, the aperture is 75 μ m-32 μ m.
8. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that the described electron microscope enlargement factor of step 3 from 30-1000 doubly.
9. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that the described polarizing microscope enlargement factor of step 3 from 20-200 doubly.
10. according to the detection conclusive evidence method of asbestos in right 1 described a kind of talcum powder and the talcum powder, it is characterized in that the described microscopic examination method of step 3 is length-diameter ratio greater than 3 mineral fibres to the judgment basis of asbestos.
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Cited By (4)
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| CN106338424A (en) * | 2015-07-10 | 2017-01-18 | 中国石油化工股份有限公司 | Method for analyzing clay mineral in rock sample with high quartz content |
| 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 |
| 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 |
| CN113092507A (en) * | 2021-03-19 | 2021-07-09 | 四川大学 | High-efficiency intelligent identification and analysis method for microstructure of material |
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Cited By (4)
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Application publication date: 20130925 |