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GB 24613-2009 English PDF

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GB 24613-2009: Limit of harmful substances of coatings for toys
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Standard similar to GB 24613-2009

GB 24409   GB/T 24147   GB/T 23999   GB 30981.2   GB 30981.1   GB 18581   

Basic data

Standard ID GB 24613-2009 (GB24613-2009)
Description (Translated English) Limit of harmful substances of coatings for toys
Sector / Industry National Standard
Classification of Chinese Standard G51
Classification of International Standard 87.040
Word Count Estimation 25,290
Date of Issue 2009-11-15
Date of Implementation 2010-10-01
Quoted Standard GB/T 1250; GB/T 1725-2007; GB/T 3186; GB/T 6682; GB/T 6750-2007; GB/T 9750
Regulation (derived from) Announcement of Newly Approved National Standards No. 13 of 2009 (No. 153 overall)
Issuing agency(ies) General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China
Summary This Chinese standard specifies the toys with paint on substances harmful to humans and the environment to allow limited requirements, test methods, inspection rules and signs, etc. Package Contents. This standard applies to all kinds of toys with paint.

GB 24613-2009: Limit of harmful substances of coatings for toys

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Limit of harmful substances of coatings for toys ICS 87.040 G51 National Standards of People's Republic of China Toys with paint of harmful substances Posted 2009-11-15 2010-10-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released

Table of Contents

Introduction Ⅲ 1 Scope 1 2 Normative references 1 3 Terms and definitions 4 Requirements 1 5 Test Method 2 6 Inspection rules 2 7 Package mark 3 Determination of Appendix A (normative) lead content of 4 Determination of Appendix B (normative) content of soluble elements 7 (Normative) Determination of phthalates in Appendix C --- GC-MS 10 Determination of Annex D (normative) volatile organic compounds (VOC) content of 15 Determination of benzene, toluene, ethylbenzene and xylene content of Appendix E (normative) 19

Foreword

All the technical contents of this standard is mandatory. The Standard Appendix A, Appendix B, Appendix C, Appendix D, Appendix E are normative appendices. The standard proposed by China Petroleum and Chemical Industry Association. This standard by the National Standardization Technical Committee paint pigment. This standard was drafted. CNOOC Changzhou coating Chemical Research Institute, China Paint (Shenzhen) Co., Ltd., Shenzhen Song Hui Chemical Co., Ltd. Hengchang Petrochemical Co., Ltd., Zhejiang Huanda Paint Industry Group Co., Ltd., Guangdong Carpoly Chemical Co., Ltd., Hangzhou Paint Co., Ltd., Jiangsu Su Changjiang Paint Co., Ltd., Shanghai Fu-chen Chemical Co., BASF (China) Co., Ltd. Kunshan City Shiming Technology Development Co., Paint Co., Ltd. Changzhou City, Su Lei. The main drafters of this standard. Huang Ning, runner-up Wang, Wang Zhi, Zhang Dingde, Hu Guanghui, Qiu Yuqing, Xu promising, Jiang Fang Qun, Zhang Haojun, Chenshou Sheng, Yuyun table, Lv Shiming, Weisu Qin. Toys with paint of harmful substances

1 Scope

This standard specifies the toys with paint of harmful substances to humans and the environment to allow limited requirements, test methods, inspection rules and packaging Signs and so on. This standard applies to all types of toys with paint.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard. Representation GB/T 1250 limit values and the method of determining GB/T 1725-2007 Paints, varnishes and plastics - Determination of volatile matter content is not (ISO 3251.2003, IDT) GB/T 3186 Paints, varnishes and raw materials for paints and varnishes - Sampling (GB/T 3186-2006, ISO 15528.2000, IDT) GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD) GB/T 6750-2007 Paints and varnishes - Determination of density - Pycnometer method (ISO 2811-1.1997, Paintsand varnishes-Determinationofdensity-Part 1. Pyknometermethod, IDT) GB/T 9750 product packaging and marking paint

3 Terms and Definitions

The following terms and definitions apply to this standard. 3.1 Toys can be coated on the surface to form a coating liquid or solid coatings in general. 3.2 101.3kPa at standard atmospheric pressure, any initial boiling point equal to or lower than the organic compound 250 ℃. 3.3 Prescribed method of test product obtained VOC content.

4 Requirements

Products harmful substances shall comply with the requirements of Table 1. Table 1 harmful substances requirements Project Requirements Lead content of a/(mg/kg) ≤ 600 Content of soluble elements a/(mg/kg) ≤ Antimony (Sb) 60 Arsenic (As) 25 Barium (Ba) 1000 Table 1 (continued) Project Requirements Content of soluble elements a/(mg/kg) ≤ Cadmium (Cd) 75 Chromium (Cr) 60 Lead (Pb) 90 Mercury (Hg) 60 Selenium (Se) 500 Phthalate content b /% ≤ Iso-octyl phthalate (DEHP), Dibutyl phthalate (DBP) and O sum of butyl benzyl phthalate (BBP) 0.1 Diisononyl phthalate (DINP), Diisodecyl phthalate (DIDP) and Total octyl phthalate (DNOP) 0.1 Volatile organic compound (VOC) content of c/(g/L) ≤ 720 Benzene content c /% ≤ 0.3 Toluene, ethylbenzene and xylene content of the sum of c /% ≤ 30 a by product EXPRESS construction ratio (without thinner added) mixed sample preparation, and preparation of appropriate thickness of the coating. Dried product instructions provided Under the conditions, to be completely dry coating, dry film was measured. Powder coating directly measured. b liquid sample, by product EXPRESS construction ratio to prepare a mixed sample, press a predetermined measurement method of the content, and then converted to the content of the dried film. powder Like the end sample or samples dried film, its content was determined by the method specified. c applies only to solvent-based coatings. By product EXPRESS mixing ratio was measured after construction. Such as the use of a range of the amount of diluent should be in accordance with the recommended After the determination of the maximum amount of dilution dilution.

5 Test methods

5.1 Sampling Product sampling as prescribed by GB/T 3186 will be. 5.2 inspection method 5.2.1 Determination of lead content in accordance with the standards set forth in Appendix A be. 5.2.2 Determination of soluble elements according to the standards set forth in Appendix B will be. 5.2.3 Determination of phthalates in accordance with the standards set forth in Appendix C of conduct. 5.2.4 Determination of volatile organic compounds according to the standards in Appendix D of the regulations. 5.2.5 benzene and toluene, ethylbenzene and xylene was measured by the sum of the provisions of Appendix E of this standard will be.

6 Inspection rules

6.1 standard listed all the requirements of both types of test items. 6.1.1 Under normal production conditions, type inspection at least once a year. 6.1.2 There should be one of the following type test at any time. --- Original shape when the new product; --- Products produced at different places; --- Production formula, process, key sources of raw materials and products construction ratio when there is a greater change; --- Discontinued after three months to resume production when. 6.2 determination of test results 6.2.1 The test results determined in accordance with GB/T 1250 in the rounding value comparison method. After rounding the test results of 0, 0.0, the results One significant figure reported. 6.2.2 should be reported test results also indicate the product expressly construction ratio. 6.2.3 Test results of all items meet the requirements of this standard, the product to comply with the requirements of this standard.

7 Package mark

7.1 Product packaging and marking shall comply with the provisions of GB/T 9750 outside, according to the standard test qualified products can be expressed in the packaging logo. 7.2 For the two-component or multi-component coating by a supporting component, packaging, logo or product specification should be clear construction ratio of each component. The need for the construction diluted paints, packaging or labeling product specification should be clear dilution ratio.

Appendix A

(Normative) Determination of lead content A. Rationale After drying the coating using a suitable method to remove all organic material, and the use of appropriate analytical instruments Test Solution Lead content. A. 2 Reagents Analysis and testing use only recognized as analytical reagent, the water in line with GB/T 6682 in the three water requirements. A. 2.1 Nitric acid. about 65% (by mass) density of about 1.40g/mL, nitric acid should not be used already yellowing. A. 2.2 Hydrogen peroxide. about 30% (by mass) density of about 1.10g/mL. A. 2.3 magnesium carbonate. A. 2.4 nitric acid solution a 1. 1 (volume ratio). A. 2.5 nitric acid solution. two ninety-eight (volume ratio). A. 2.6 lead standard stock solution. a concentration of 100mg/L or 1000mg/L. A. 3 instruments and equipment Common laboratory equipment as well as some of the following equipment. A. 3.1 appropriate analytical instruments. such as flame atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometer. A. 3.2 crushing equipment. shredders, scissors or other suitable grinding equipment. A. 3.3 Electric hot plate. Temperature-controlled. A. 3.4 muffle furnace. the temperature can be controlled at (475 ± 25) ℃. A. 3.5 microwave digestion. A. 3.6 Balance. Precision 0.1mg. A. 3.7 crucible; 50mL. A. 3.8 Beaker. 50mL. A. 3.9 membranes (for water). Aperture 0.45μm. A. 3.10 flask. 50mL, 100mL like. A. 3.11 pipettes. 1mL, 2mL, 5mL, 10mL, 25mL and the like. A. 3.12 glass or Teflon plate. All glassware, sample containers, glass or Teflon boards are required before using a nitric acid solution (A.2.4) soaking 24h, and then thoroughly washed with water and dried. A. 4 Test Procedure A. 4.1 Preparation of coating Stir sample to be tested. By product EXPRESS construction ratio (without thinner added) to prepare a mixed sample, stir in Bolivia Suitable coating thickness glass plate or PTFE plate (A.3.12) prepared on. Product under dry conditions specified in the instructions, until the film has completely Drying [since the dry paint if drying temperatures not exceeding (60 ± 2) ℃], remove the film, at room temperature with a crushing device (A.3.2) will be crushed, The coating film is smaller than 5mm. Note 1. The coating film can not be crushed (such as elastic or plastic film), use a clean pair of scissors (A.3.2) the film was cut, the coating is smaller than 5mm. Note 2. The powder samples, sample directly. A. 4.2 Sample Preparation Sample preparation for the second parallel testing. This standard provides the following three sample digestion methods, the laboratory can choose one depending on the conditions. A. 4.2.1 dry ashing method Said pulverized samples taken from about 0.2g ~ 0.3g (accurate to 0.1mg) into a crucible (A.3.7) inside, about 0.5g magnesium carbonate (A.2.3) covering the sample crucible. The crucible was placed on a hot plate inside a fume hood (A.3.3) on gradually raising the temperature of the heating plate (No more than 475 ℃) until the sample is digested to a charred mass and the volatile decomposition products have been fully discharged, leaving only a dry carbonaceous residue. However After the crucible into the (475 ± 25) ℃ in muffle furnace (A.3.4) in the insulation until completely gray. Ashing period shall supply sufficient air oxidation, but the substance is not allowed in the crucible at any stage of combustion occurs. To be filled with the ash of the crucible after cooling to room temperature, 5mL nitric acid (A.2.1), and then the solution in the crucible with a filter (A.3.9), filtered and transferred to a 50mL volumetric flask (A.3.10), and washed with water and filter crucible, and the resulting solution was collected in all the same A volumetric flask and dilute to the mark. At the same reagent blank test. Note. This method does not apply to the fluorocarbon coating. A. 4.2.2 Wet acid digestion He said pulverized samples taken from about 0.1g ~ 0.3g (accurate to 0.1mg) a 50mL beaker (A.3.8), and nitric acid was added 7mL (A.2.1), at the mouth of the beaker stamped a Petri dish on a hot plate (A.3.3) heating the solution was kept on a boil for about 15min, continue to increase Heat until white fumes. The beaker was removed from the hot plate, cool for approximately 5min, was slowly added dropwise 1mL ~ 2mL hydrogen peroxide (A.2.2 The) three Times. Calm and join other reactions required after each addition. The beaker was again placed on a hot plate heated to sample digestion completely. Such kind Incomplete digestion product, remove the coolish, then add the appropriate amount of concentrated nitric acid (A.2.1) and hydrogen peroxide (A.2.2) 1 ~ 2 times, continue heating the sample consumption Complete solution. Residual solution to about 1mL, remove the beaker to cool to room temperature. With approximately 10mL diluted with water, then with membrane (A.3.9) The solution was filtered and transferred to a 50mL volumetric flask (A.3.10) in. Rinse the beaker and the membrane, the resulting solution is all collected in the same Volumetric flask and dilute to the mark. At the same reagent blank test. A. 4.2.3 Microwave Digestion He said pulverized samples taken from about 0.1g ~ 0.2g (accurate to 0.1mg) placed in a microwave digestion vessel were added 5mL nitric acid (A.2.1) and 2mL hydrogen peroxide (A.2.2), and then the digestion tank closed. According to the following procedure digestion temperature. raised in about 10min (180 ± 5) ℃, 30min maintaining the temperature after cooling. After digestion vessel was cooled to room temperature, open the digestion tank, the digestion solution through a membrane filter (A.3.9), filtered and transferred to a 50mL volumetric flask (A.3.10) in. Rinse the inner tank digestion and an inner lid, the washing liquid is collected in the same Volumetric flask, and filters are rinsed with water, the resulting solution was collected in all the same volumetric flask and dilute to the mark. While doing Reagent blank test. When using the above sample digestion method can determine the appropriate digestion conditions based on the actual situation of the sample to ensure that the sample of organic All compounds were removed, and the dissolution of all measured elements. If the sample is treated to have residue, residue use appropriate measurements [such as X Ray fluorescence spectrometry (XRF)] was measured, tested to ensure no element exists. Otherwise it should be changed so that the measured element digestion conditions completely dissolved. Digestion solution was testing should be completed within 24h, otherwise the application of nitric acid (A.2.1) to be stable, so that concentration saved Ba (of HNO3) about 1mol/L. A. 4.3 Test Press A. 4.2 Preparation of test solution using appropriate analytical instruments (A.3.1) Determination of lead content. When using any of the instruments were measured, the analyst should be in accordance with the manufacturer's instructions or the operating manual and its operating Test, and indicate the use of analytical instrumentation in the test report. A. 5 calculation results According to formula (A.1) to calculate the sample Lead content. (Ρ-ρ0) Vp × F (A.1) Where. --- Samples lead content in milligrams per kilogram (mg/kg); ρ --- test solution lead concentration in milligrams per liter (mg/L); ρ0 --- blank solution lead concentration in milligrams per liter (mg/L); Volume Vp --- test solution, in milliliters (mL); F --- the test dilution of the solution; A. 6 precision A. 6.1 Repeatability The same operator to double the relative deviation of the test results should be less than 10%. A. 6.2 Reproducibility Relative deviations between different laboratories test results should be less than 20%.

Appendix B

(Normative) Determination of the content of soluble elements B. Rationale After coating with 0.07mol/L hydrochloric acid solution treated and dried using an appropriate analytical instrument detection limit of the test solution was measured soluble yuan Pigment content. B. 2 Reagents Analysis and testing use only recognized as analytical reagent, the water in line with GB/T 6682 in the three water requirements. B. 2.1 HCl. about 37% (by mass) density of about 1.18g/mL. B. 2.2 hydrochloric acid solution. 0.07mol/L. B. 2.3 hydrochloric acid solution. approximately 2mol/L. B. 2.4 nitric acid solution a 1. 1 (volume ratio). B. 2.5 antimony, arsenic, barium, cadmium, chromium, lead, mercury, selenium standard stock solution. a concentration of 100mg/L or 1000mg/L. B. 3 instruments and equipment Common laboratory equipment as well as some of the following equipment. B. 3.1 The detection limit appropriate (see B.6) analytical instruments (such as atomic absorption spectroscopy, inductively coupled plasma atomic emission spectrometer). B. 3.2 crushing equipment. shredders, scissors and so on. B. 3.3 stainless steel metal sieve. aperture of 0.5mm. B. 3.4 Balance. Precision 0.1mg. B. 3.5 Heating and stirring device. the device should be in a constant temperature (37 ± 2) ℃ and continuous automatic mixing, stirring or outer layer should be polytetrafluoroethylene glass. It can also be used in a constant temperature (37 ± 2) ℃ in shaking water bath. B. 3.6 pH meter. accuracy of ± 0.2pH units. B. 3.7 membranes (for water). Aperture 0.45μm. B. 3.8 flask. 25mL, 50mL, 100mL like. B. 3.9 Pipette. 1mL, 2mL, 5mL, 10mL, 25mL, 50mL and the like. B. 3.10 series of chemical containers. total capacity of hydrochloric acid solution (to B.2.2) extractant volume of 1.6 to 5.0 times. B. 3.11 glass or Teflon plate. All glassware, sample containers, stirring, glass or Teflon boards are required before using a nitric acid solution (B.2.4) Soak 24h, then washed with water and dried. B. 4 Test Procedure B. 4.1 Preparation of coating Stir sample to be tested. By product EXPRESS construction ratio (without thinner added) to prepare a mixed sample, stir in Bolivia Suitable coating thickness glass plate or PTFE plate (B.3.11) prepared on. Product under dry conditions specified in the instructions, until the film has completely Drying [since the dry paint if drying temperatures not exceeding (60 ± 2) ℃], remove the film, at room temperature with a crushing device (B.3.2) will be crushed, With stainless steel mesh (B.3.3) sieved to be treated. Note 1. The coating film can not be crushed (such as elastic or plastic film), use a clean pair of scissors (B.3.2) as the film was cut without sifting directly Sample handling. Note 2. The powder samples, sample directly. B. 4.2 Sample Preparation Sample preparation for the second parallel testing. Using a suitable chemical containers (B.3.10), with a suitable pipette (B.3.9) will be equivalent to 50 times the quality of the test sample, temperature (37 ± 2) ℃ of hydrochloric acid solution (B.2.2) is mixed with the test sample. On stirring device (B.3.5) After stirring for 1min, acidimeter (B.3.6) measure its acidity. If the pH is > 1.5, while stirring the mixture, a solution of hydrochloric acid was added dropwise while (. B.2.3) [If the test sample Sample contains a large amount of alkaline carbonate compounds can be added dropwise hydrochloric acid (B.2.1)] to adjust the pH value between 1.0 to 1.5. Mixed It was dark, and then in the (37 ± 2) ℃ under continuous stirring 1h, then at (37 ± 2) ℃ placed 1h, followed immediately by filtration through a membrane filter (B.3.7). The filtrate was filtered stored in the dark and should be complete elemental analysis within 24h. If the filtrate While saving elemental analysis before Among more than 24h, you should use hydrochloric acid (B.2.1) to be stable, so that saved Ba concentration (HCl) about 1mol/L. NOTE. Throughout the extraction period, the speed of the stirrer should be adjusted to maintain the sample is always in a suspended state, and should try to avoid spills. B. 4.3 Test Press B. 4.2 Preparation of test solution using appropriate detection limits (see B.6) analytical instruments (B.3.1) measured soluble harmful elements content. When using any of the instruments were measured, the analyst should be in accordance with the manufacturer's instructions or the operating manual and its operating Test, and indicate the use of analytical instrumentation in the test report. B. 5 calculation results B. 5.1 according to formula (B.1) content in the sample were calculated in a variety of soluble elements. (Ρ-ρ0) Vp × F (B.1) Where. --- Soluble elements content of the sample, in units of milligrams per kilogram (mg/kg); Ρ --- measuring the concentration of the test solution, in milligrams per liter (mg/L); ρ0 --- blank solution (A.2.2) the determination of the concentration, in milligrams per liter (mg/L); Vp --- volume of test solution volume in milliliters (mL); F --- the test dilution of the solution; B. 5.2 Calibration results Due to the accuracy of this test method, when considering the test results between laboratories, to be corrected obtain the final results of the analysis. which is Formula (B.1) in the calculation of results should subtract the result is multiplied Table B. 1 Value Analysis correction coefficient corresponding elements as the final element The results reported. Table B. A correction coefficient of each element analysis Element antimony (Sb) Arsenic (As), barium (Ba) Cadmium (Cd) Chromium (Cr) Lead (Pb) Mercury (Hg) selenium (Se) Analysis of the correction coefficient /% 6,060,303,030,305,060 Example. The results lead to 120mg/kg, the analysis of lead in the correction coefficient table 1 is 30%, the final results of the analysis = (120-120 × 30%) mg/kg = 84mg/kg. B. The detection limit of the test method 6 Determination of soluble elements of the above analysis, the detection limit should not exceed one-tenth of a limited amount of the element. Analysis of the test side Detection limit is generally considered to be the blank test three times the standard deviation. Above the blank value was determined by laboratory tests. B. 7 precision B. 7.1 Repeatability Same operator twice the relative deviation of the test results should be less than 20%. B. 7.2 Reproducibility Relative deviations between different laboratories test results should be less than 33%.

Appendix C

(Normative) Determination of phthalate esters --- GC-MS C. Rationale Methyl ethyl ketone solvent in a sample of phthalates ultrasonic extraction. After the volume of extract, GC/MS with Instrument (GC-MS) assay. With full scan total ion chromatogram (TIC) and mass spectra (MS) qualitative and selected ion monitoring (SIM) And external standard method for quantitative. C. Materials and Reagents C. 2.1 Carrier gas. helium, purity ≥99.999%. C. 2.2 Dilution solvent. methyl ethyl ketone, purity (mass fraction) ≥99% purity or known. C. 2.3 Calibration compound. dibutyl phthalate (DBP), phthalate, butyl benzyl phthalate (BBP), di-iso-octyl phthalate (DEHP), dibutyl phthalate octyl phthalate (DNOP), diisononyl phthalate (DINP), diisodecyl phthalate (DIDP), pure Degree (mass fraction) ≥98% purity or known. C. 2.4 standard stock solution. namely, accurately weighed amount of phthalates calibration compound (C.2.3), formulated with butanone (C.2.2) A concentration of standard stock solution of 5000mg/L of. NOTE. The standard stock solution (0 ~ 4) ℃ refrigerator, valid for six months. C. 2.5 mixed standard working solution. using serial dilution method, diluting the standard stock solution (C.2.4) with butanone (C.2.2) to apply concentrated Mixed standard working solution degrees. NOTE. The standard working solution (0 ~ 4) ℃ refrigerator, valid for three months. C. 3 instruments and equipment C. 3.1 Gas chromatography/mass spectrometry (GC-MS). C. 3.2 Injector. capacity should be at least twice the amount of injection. C. 3.3 Vial. Approximately 10mL bottles, with sealable cap. C. 3.5 flask. 50mL, 100mL like. C. 3.6 stoppered conical flask. 50mL like. C. 3.7 crushing equipment. shredders, scissors or other suitable grinding equipment. C. 3.8 ultrasonic generator. power 500W. C. 3.9 membranes (for organic solvents). Aperture 0.45μm. C. 3.10 balance. accuracy 0.1mg. NOTE. phthalates are common contaminants in the laboratory, reagents, solvents and glassware etc. Phthalates may be contaminated, causing dry Interference. Therefore, the analysis process, avoid using plastic containers. In addition, the glassware before use, must be placed in a high temperature oven baked to 400 ℃ 2h ~ 4h, or analytically pure solvent rinse. C. 4 Gas chromatography - mass spectrometry test conditions Column. 5% diphenyl/95% dimethyl polysiloxane capillary column, 30m × 0.25mm × 0.25μm, for example. DB-5MS hair Fine column. Column temperature. initial temperature 60 ℃ maintained 0.75min, then 30 ℃/min was raised to 180 ℃, 1min, to then to 15 ℃/min l To 280 ℃, holding 7min; Inlet temperature. 280 ℃; Chromatography - mass spectrometry interface temperature. 280 ℃; Ion source temperature. 230 ℃; Carrier gas flow rate. 1.0mL/min; Injection mode. splitless, 0.75min after the valve opening; Injection volume. 1.0μL; Ionization mode. EI; Ionization Energy. 70eV; Measurement method. full-scan total ion chromatogram (TIC) and mass spectra (MS) qualitat...

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