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GB/T 23263-2009 English PDF (GBT23263-2009)

GB/T 23263-2009 English PDF (GBT23263-2009)

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GB/T 23263-2009: Determination of asbestos in products

This Standard specifies the test method for the determination of asbestos in products using powder X-ray diffractometer and polarizing microscope. This Standard applies to the determination of asbestos in building materials, friction materials, sealing materials, heat insulating materials, and non-metallic minerals.
GB/T 23263-2009
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 73.080
Q 61
Determination of asbestos in products
ISSUED ON. MARCH 09, 2009
IMPLEMENTED ON. NOVEMBER 05, 2009
Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the PRC;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms, symbols, and units ... 4
4 Test method and principle ... 6
5 Sampling ... 10
6 Preparation method of the first analysis sample ... 11
7 Qualitative analysis method based on the first analysis sample ... 12 8 Judgement method for presence of asbestos ... 19
9 Preparation methods of the second analysis sample and the third analysis sample for quantitation ... 20
10 X-ray diffraction quantitative analysis method based on base standard absorption correction method ... 21
11 Report of test results ... 25
Appendix A (Normative) Technical conditions for the powder X-ray
diffractometer when determining asbestos ... 27
Appendix B (Normative) Specification of polarizing microscope ... 29
Appendix C (Normative) Base standard absorption correction method relating to asbestos ... 30
Determination of asbestos in products
1 Scope
This Standard specifies the test method for the determination of asbestos in products using powder X-ray diffractometer and polarizing microscope.
This Standard applies to the determination of asbestos in building materials, friction materials, sealing materials, heat insulating materials, and non-metallic minerals.
2 Normative references
The following documents contain provisions which, through reference in this Standard, constitute provisions of this Standard. For the dated references, their subsequent amendments (excluding corrections) or revisions do not apply to this Standard. However, the parties who enter into agreement based on this Standard are encouraged to investigate whether the latest editions of these documents are applicable. For undated reference documents, the latest
editions apply to this Standard.
GB 10736 Chemical - Potassium chloride
GB/T 15896 Chemical reagent - Formic acid
HG/T 2892 Chemical reagent - Isopropyl alcohol
3 Terms, symbols, and units
3.1 Terms and definitions
The following terms and definitions apply to this Standard.
3.1.1 Asbestos
Fibrous silicate mineral (chrysotile) belonging to serpentine group and fibrous silicate mineral (amosite, crocidolite, tremolite, actinolite, anthophyllite) belonging to amphibole group among the minerals which constitute rock.
3.1.2 Vermiculite
Mica group swelling clay mineral. The structural layer contains a layer of internal standard method and standard addition method. These methods are not very accurate in asbestos analysis, but can be used as the methods for judging the approximate asbestos content.
5 Sampling
5.1 Sampling method
5.1.1 The protective measures shall be taken so that the persons involved in sampling do not inhale asbestos dust at the time of sampling.
5.1.2 In the case of sampling at job site, care shall be taken so that the present condition is not disturbed. Sampling is carried out by using a sharp knife and the like. Care shall also be taken so that asbestos dust is not scattered. 5.1.3 In the case of sampling from products, the sample representing the lot is taken.
5.1.4 The size of sample shall be the sufficiently large so that it represents the product to be measured. In the case of soft materials such as spraying material, or heat insulating material, the sample of approximately 10 cm3/place is taken at three places. In the case of board shaped and rigid material, the sample of approximately 10 cm2/place is taken at three places.
5.2 Transportation and storage of sample
The transportation of the sample from the sampling place to the place of analysis shall be carried out by putting the sample in a hermetically-sealed container to avoid dust scattering.
5.3 Sampling record
For the sample taken, the necessary items are recorded for discrimination. a) Name of product;
b) Sampled position and place;
c) Sample information. shape, material, sample area, sample quantity,
sampling method, and sampling date;
d) Sampler.
Where.
ma - The mass of sample and crucible before heat treatment, in grams (g); mb - The mass of sample and crucible after heat treatment, in grams (g); mc - The mass of crucible, in grams (g);
m0 - The mass of sample before heat treatment, in grams (g);
m - The mass of sample after heat treatment, in grams (g).
7 Qualitative analysis method based on the first
analysis sample
7.1 Qualitative analysis method by powder X-ray diffractometer
7.1.1 The first analysis sample is placed uniformly and flat into the sample dish. The sample dish is the metallic plate or glass plate with hole or hollow. 7.1.2 For the sample dish containing the sample, according to the qualitative analysis conditions specified in Appendix A, X-ray diffraction qualitative analysis is carried out.
7.1.3 According to the X-ray diffraction pattern, it is confirmed whether the characteristic peaks of asbestos (chrysotile, amosite, crocidolite,
tremolite/actinolite, anthophyllite) as shown in Figure 4 ~ Figure 8 or of vermiculite group (hydrobiotite, vermiculite) as shown in Figure 9 ~ Figure 10 appear in the first analysis sample. The results are applied to the analysis specified in 7.2 and Clause 9.
Note. It is difficult to distinguish between tremolite and actinolite by X-ray diffraction method, so they can be classified into the same kind during analysis.
7.1.4 When it is confirmed in 7.1.3 that there is a vermiculite group diffraction characteristic peak, in accordance with the provisions of 7.3, analysis shall be carried out.
7.2.2 Determination method
7.2.2.1 PLACE the sample prepared by 7.2.1.1 or 7.2.1.2 on the stage of polarizing microscope. The specifications of polarizing microscope shall be in accordance with Appendix B.
7.2.2.2 At 10 times the objective lens, verify whether the particles are evenly dispersed.
7.2.2.3 For the sample which has been confirmed in 7.2.2.2 to be uniformly dispersed, adjust the objective lens to 40 times, to confirm whether the fiber corresponding to the dispersion color of Table 2 exists.
7.2.2.4 Under a 10 times eyepiece of the polarizing microscope, MOVE the field of view and count, until the total number of all asbestos containing fiber particle in the circle with a diameter of 100 ??m in the eyepiece counter reaches 1000. The kind and number of particles of the asbestos showing the dispersion color of Table 2 are recorded.
Note. When identifying the dispersion color, USE the analyzer which is compatible with the microscope. If the analyzer is rotated by 90?? or more, the color development state can be more easily confirmed.
7.2.2.5 If the asbestos diffraction characteristic peak appears in 7.1.3, according to the kind of asbestos, the operations of 7.2.2.1~7.2.2.4 are performed on the 3 samples respectively. If the asbestos diffraction
characteristic peak does not appear in 7.1.3, according to the kind of asbestos which may be used, the operations of 7.2.2.1~7.2.2.4 are performed on the 3 samples respectively. If asbestos is not detected by analysis of the dipping liquid showing the refractive index of sensitive color in 7.2.1.2, according to the kind of asbestos which may exist, USE a dipping liquid of refractive index other than the sensitive color shown in Table 2 to make 3 samples respectively; also perform the operations of 7.2.2.1~7.2.2.4, to reconfirm this result.
7.3 Qualitative analysis method for the vermiculite group for spraying
7.3.1 Potassium chloride treated sample
7.3.1.1 PUT 1.0 g of the first analysis sample into the beaker; POUR 100 mL of potassium chloride aqueous solution in accordance with GB 10736 at a
concentration of 1 mol/L; and evenly DISPERSE it.
7.3.1.2 At 70 ??C ~ 80 ??C, LET the beaker stand for 1 h.
7.3.1.3 After standing, USE a centrifugal separator to centrifuge and precipitate; COLLECT the precipitate and USE distilled water to wash it thoroughly.
For reanalysis, asbestos with diffraction peaks and other asbestos which may be used are taken as the objects. USE the first analysis sample; according to 7.2.1.2, MAKE a new sample for analysis.
In the results of the reanalysis, if the fiber particles of asbestos are still less than 4, it is considered that the sample does not contain asbestos. If the fiber particles of asbestos are 4 or more, it is considered that asbestos is contained in the sample; and in accordance with 8.1, quantitative analysis is carried out. 8.4 If the asbestos diffraction characteristic peaks shown in Figure 4 ~ Figure 8 do not appear in the X-ray diffraction qualitative analysis results; and in the qualitative analysis results of polarizing microscope, among the 3000 particles in total of three samples, the asbestos has less than 4 fiber particles; then it is considered that the sample does not contain asbestos.
Note. The minerals with the same X-ray diffraction characteristic peaks as chrysotile are serpentine (antigorite, lizardite), chlorite, and kaolin minerals (kaolinite, halloysite). The mineral with the same X-ray diffraction angle (9??~10??) as amosite and crocidolite is talc.
8.5 For vermiculite group for spraying, if X-ray diffraction characteristic peak of asbestos does not appear in the first analysis sample treated with potassium chloride, or the integral intensity of the characteristic peak is less than that of the standard sample, it is considered that the sample does not contain asbestos. In other cases, it is considered that the sample contains asbestos.
9 Preparation methods of the second analysis sample
and the third analysis sample for quantitation
9.1 Preparation method of the second analysis sample
9.1.1 Measure beforehand the mass of fluororesin binder glass fiber filter (hereafter referred to as ?€?filter?€?) of 25 mm diameter required for the preparation of the second analysis sample and the X-ray diffraction intensity of base standard material.
9.1.2 Weigh 100 mg (M1) of the first analysis sample precisely, put it in a conical beaker, add 20 mL of 20% formic acid and 40 mL of no dust water, and disperse them by using an ultrasonic cleaner for one minute.
9.1.3 Put it in a thermostat bath set at 30 ??C??1 ??C and repeat six times the cycle consisting of agitation for 30 s and leaving it to stand for 90 s.
9.1.4 USE an extraction filter equipped with a glass filter mat having a diameter 10.1.1.1 Measure beforehand the mass of filter required for the drawing of standard curve and the X-ray diffraction intensity.
10.1.1.2 Weigh 0.1 mg, 0.5 mg, 1.0 mg, 3.0 mg and 5.0 mg of the asbestos standard sample, put them in five conical beakers, add 0.02 mL, 0.1 mL, 0.2 mL, 0.6 mL and 1.0 mL of 20% formic acid and 0.04 mL, 0.2 mL, 0.4 mL, 1.2 mL and 2.0 mL of no dust water respectively and disperse them by using an ultrasonic cleaner for one minute.
10.1.1.3 Put them in a thermostat bath set at 30 ??C??1 ??C and repeat six times the cycle consisting of agitation for 30 s and leaving it to stand for 90 s. 10.1.1.4 USE an extraction filter equipped with a glass filter mat having a diameter of 25 mm to extract and filter, to obtain the standard curve sample. 10.1.1.5 Fix the respective samples for standard curve prepared to the sample stage of X-ray diffraction analyzing apparatus; measure the base standard plate and the X-ray diffraction intensity concerned; and prepare the standard curve according to the base standard absorption correction method based on
Appendix C. NOTE that the main diffraction intensity IZn0 of metal base standard plate shall be measured in advance in the state in which the filter is installed.
Note. The metal base plate may use one of zinc or aluminum.
10.1.2 Standard curve II method
10.1.2.1 Measure beforehand the mass of filter required for the drawing of standard curve and the X-ray diffraction intensity.
10.1.2.2 Precisely WEIGH 10 mg of asbestos standard sample into a 500 mL beaker; ADD 100 mL ~ 150 mL of isopropyl alcohol in accordance with HG/T 2892 and STIR; and USE an ultrasonic cleaner to fully disperse. Then
TRANSFER to a 1000 mL flask; continue to add isopropyl alcohol until 1000 mL is reached, as a mother liquid.
Note. 1 mL of mother liquid is equivalent to containing 0.01 mg of sample. 10.1.2.3 USE a pipette to take 3 parts of each of 5 mL, 10 mL, 30 mL, 50 mL, and 100 mL of the suspension from the mother liquid; place them in conical beakers. NOTE that the flask containing the mother liquid shall be shaken well when pipetting; and then PIPETTE immediately.
Note. In the mother liquid which is left to stand for a long time, the dispersed asbestos may precipitate, and it is necessary to visually judge whether the asbestos is evenly

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