GB/T 30157-2013 English PDF

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Basic data

Standard ID: GB/T 30157-2013 (GB/T30157-2013)
Description (Translated English): Textiles -- Determination of total content of lead and cadmium
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: W04
Classification of International Standard: 59.080.01
Word Count Estimation: 10,195
Quoted Standard: GB/T 6682
Regulation (derived from): National Standards Bulletin No. 25 of 2013
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 standard specifies the method for the determination of total lead and textile products in the total cadmium content. This standard applies to all kinds of textile products.

GB/T 30157-2013: Textiles -- Determination of total content of lead and cadmium

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Textiles. Determination of total content of lead and cadmium [Quasi-Official/Academic version - Translated by Chinese Institute] ICS 59.080.01 W04 National Standards of People's Republic of China Determination of total lead and total cadmium content in textiles Published on.2013-12-17 2014-10-15 implementation General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China China National Standardization Administration released

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard is proposed by the China Textile Industry Federation. This standard is under the jurisdiction of the Technical Committee on Basic Standards of the National Textile Standardization Technical Committee (SAC/TC209/SC1). This standard was drafted by. China Textile Standard (Beijing) Inspection & Certification Center Co., Ltd., National Textile Product Quality Supervision and Inspection Center, Chinese Republic of China Ningbo Entry-Exit Inspection and Quarantine Bureau. The main drafters of this standard. Zhang Hui, Jing Tingting, Zheng Yuxiu, Bao Qijun, Feng Yun, Fu Kejie. Determination of total lead and total cadmium content in textiles Warning. Persons using this standard should have practical experience in regular laboratory work. This standard does not indicate all possible security issues. It is the user's responsibility to take appropriate safety and health measures and to ensure compliance with the conditions set by the relevant national laws and regulations.

1 Scope

This standard specifies the method for the determination of total lead and total cadmium in textile products. This standard applies to all kinds of textile products.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article Pieces. For undated references, the latest version (including all amendments) applies to this document. GB/T 6682 Analysis Laboratory Water Specifications and Test Methods

3 Principle

The sample is digested with concentrated acid, and the digested solution is diluted to volume and then inductively coupled plasma emission spectrometer (ICP-AES) is used. The emission intensity of lead and cadmium is measured under the conditions, or the absorbance of lead and cadmium is measured with an atomic absorption spectrophotometer. Determine the concentration of various metal ions and calculate the total amount of heavy metals in the sample.

4 Reagents and materials

Unless otherwise stated, use only reagents of analytical grade or above and water of Grade 2 or above specified in GB/T 6682. 4.1 Concentrated nitric acid 4.2 3% (volume fraction) nitric acid Take 3mL of concentrated nitric acid (4.1) and dilute to 100mL with secondary water. 4.3 Fluoroboric acid 4.4 Hydrofluoric acid 4.5 Hydrogen peroxide 4.6 standard stock solution Standard stock solutions for each element can be prepared using standard materials or as follows. 4.6.1 Lead (Pb) Standard Stock Solution (1000μg/mL) Weigh 0.160 g of lead nitrate [Pb(NO3)2], dissolve with 10 mL of nitric acid (1 9), transfer to a 100 mL volumetric flask and dilute to the mark. 4.6.2 Cadmium (Cd) Standard Stock Solution (1000μg/mL) Weigh 0.203g of cadmium chloride (CdCl2· 2H2O ), dissolve with 10mL nitric acid (1 9), transfer to 100mL volumetric flask, dilute to Scale. Note. Unless otherwise specified, the standard stock solution has a shelf life of 6 months at room temperature (15°C~25°C). When turbidity, precipitation or color change occurs, etc. It should be re-prepared. 4.7 standard working solution (50μg/mL) Accurately pipette 2.50 mL from the standard stock solution into a volumetric flask and dilute to 50 mL with 3% nitric acid (4.2). Note. The standard working solution is generally valid for two weeks at room temperature (15°C~25°C). If turbidity, sedimentation, or color change occurs, it should be renewed. preparation.

5 Equipment and Instruments

5.1 Inductively Coupled Plasma Optical Emission Spectrometer (ICP-AES) or Atomic Absorption Spectrophotometer. 5.2 microwave digestion instrument. with program temperature control function. 5.3 digestion container. 5.4 disposable blade. 5.5 Volumetric flask. 50 mL, 100 mL. 5.6 Pipette. 0.5 mL, 1.0 mL, 2.0 mL. 5.7 Aqueous filtration membrane. 0.45 μm pore size. 5.8 Balance. The accuracy is 0.01mg.

6 Analysis steps

6.1 Preparation and Processing of Samples 6.1.1 Preparation Take a representative sample, cut the sample to a small piece of 5mm × 5mm, weigh about 0.2g sample, accurate to 0.0001g. 6.1.2 Resolution Add 5.0 mL of concentrated nitric acid (4.1) to the digestion vessel containing the sample and blank to be tested, and wait for the reaction of the sample and acid at room temperature. Afterwards, the digestion vessel was sealed and placed in a microwave digestion apparatus (5.2), warmed to (175±5) °C in 10 min, and maintained at (175±5) °C. Hold for 5 min and allow the sample to cool for at least 5 min before removing it from the microwave digestion apparatus. Before opening the digestion vessel, microwaves should be introduced in the fume hood Digest the tank to cool to room temperature or cool for at least 30 minutes. Note 1. Due to the different types of digester, different laboratories can use different digestion procedures, as long as the sample digestion is complete. Note 2. For coating samples that are difficult to digest such as PU, appropriate amounts of fluoroboric acid, hydrofluoric acid, and hydrogen peroxide may be added. Note 3. If hydrofluoric acid is used during the test, add 30 mL of 4% boric acid to each container and complex it with hydrofluoric acid to protect the quartz plasma rectangular tube. 6.1.3 sample solution to volume Transfer the digested solution to a 50 mL volumetric flask (5.5). Rinse the digestion vessel with a small amount of water 3 times. Combine the eluent in the volume. In the volumetric flask, make up to volume with water, mix, pass the aqueous phase filter membrane (5.7), the filtrate should be used as soon as possible for inductively coupled plasma emission spectrometer (ICP-AES) or atomic absorption spectrophotometer (5.1) analysis. Note. Refer to Appendix A for pretreatment methods for accessories and decorative parts for textile products. 6.2 ICP-AES analysis and determination 6.2.1 Analysis wavelength of ICP-AES analysis elements The Pb element analysis wavelength is 220.3 nm and the Cd element analysis wavelength is 214.4 nm. Note. In order to eliminate the spectral interference of other elements, you can also select a spectral line at a different wavelength for reference. 6.2.2 Determination 6.2.2.1 Determination of working curve According to test requirements and instrument conditions, the standard working solution (4.7) is gradually diluted with water to a suitable concentration of working solution. Analytical conditions of the instrument, igniting the plasma flame distance. After the flame distance is stable, at the corresponding wavelength, the concentration is measured from low to high. Spectral intensity of each element in the working solution. Taking the spectral intensity as the ordinate and the element concentration (μg/mL) as the abscissa, drawing work curve. 6.2.2.2 Determination of sample solution Determine the spectral intensity of each element in the blank solution and sample solution (6.1.3) according to the instrument conditions set in 6.2.2.1, from the working curve Calculate the concentration of each element to be measured. Note 1. If the concentration of lead and cadmium in the sample solution exceeds 1.5 times the highest point of the standard curve, the sample solution should be appropriately diluted and reanalyzed. Note 2. When determining the lead and cadmium concentration in blank solutions and sample solutions, flame atomic absorption spectrometry may also be used. When using this method, attention should be paid to the possibility of correction. The interference. The report should indicate the method used. Note 3. The analysis conditions of different instruments may be different. See Appendix B for the working conditions of some ICP spectrometers and the analytical wavelengths of the elements to be measured. 6.2.2.3 Quality Inspection The quality calibration curve should be done after every 20 test tests to ensure the accuracy of the test results.

7 result calculation

7.1 The content of heavy metal element i in the sample is calculated according to formula (1). Wi= (ci-c0)×V (1) In the formula. Wi --- the total content of heavy metals in the sample i, in milligrams per kilogram (mg/kg); Ci --- The mass concentration of the measured heavy metal i in the sample fluid, in micrograms per milliliter (μg/mL); C0 --- The mass concentration of the measured heavy metal i in the blank solution, in micrograms per milliliter (μg/mL); V --- the total volume of sample solution in milliliters (mL); m --- The mass of the sample in grams (g). 7.2 Calculation results are expressed to single digits. Below the lower limit of measurement, the test result is not detected.

8 Determination of low limit and precision

8.1 Method Detection Limit The detection limit of lead in this method was 2.50 mg/kg, and the detection limit of cadmium was 0.25 mg/kg. If using flame atomic absorption spectrometry Analysis, method detection limit may be different. 8.2 Precision In the same laboratory, the same operator uses the same equipment, according to the same test method, and in the short time to the same object The relative standard deviation of the results of two independent tests obtained independently of one another is not greater than 10%. Greater than these two measured values The condition of 10% of the arithmetic average does not exceed 5%.

9 Test report

At a minimum, the test report should give the following. a) the standard used (ie this standard) number; b) sample source and description; c) test results; d) any deviation from the details of this standard; e) Test date.

Appendix A

(Informative Appendix) Pretreatment methods for accessories and decorative parts for textile products A.1 Reagents A.1.1 Reagents listed in Chapter 4. A.1.2 Concentrated hydrochloric acid. A.2 Instruments and Equipment A.2.1 The instruments and equipment listed in Chapter 5. A.2.2 Metal cutters. A.2.3 Rotary mill. A.2.4 cryogenic mill. A.3 Analysis Procedure A.3.1 Sample Preparation A.3.1.1 Preparation of coated samples Use a disposable blade to scrape off the surface coating, do not scrape off the substrate, weigh the scraped coating 20mg ~ 100mg as a sample, accurate to 0.1mg, placed in a microwave digestion vessel (5.3) and treated according to 6.1.2 ~ 6.1.3. A.3.1.2 Preparation of Uncoated Samples A.3.1.2.1 Metal materials The sample was minced with a metal cutter (A.2.2) or the metal was ground with a rotary mill (A.2.3). Weigh 30mg~100mg test Samples, accurate to 0.1 mg, were placed in a microwave digestion vessel (5.3). Add 4.5 mL of concentrated nitric acid (4.1) and 1.5 mL of concentrated hydrochloric acid (A.1.2) to the digestion vessel containing the sample and blank to be tested. After the reaction between the sample and the acid is complete, the digestion vessel is sealed and placed in a microwave digestion apparatus (5.2), and the temperature is raised to (175±5)°C over 5.5 minutes, and Hold at (175±5)°C for 4.5 min. Allow the sample to cool for at least 5 min before removing it from the microwave digestion apparatus. Before opening the digestion vessel, it should be Cool the microwave digestion tank to room temperature or cool it for at least 30 minutes in a fume hood. Transfer the digested solution to a suitable volumetric flask (5.5) according to the size of the sample. Rinse the digestion vessel with a small amount of water and combine. Eluent in a volumetric flask, dilute to volume with water, mix, pass the aqueous phase filter (5.7), the liquid using ICP-AES or atomic absorption spectroscopy Meter (5.1) Analysis and Determination (6.2). Note. Under normal circumstances, when the sample size is 20mg ~ 49mg, transfer the digested solution in a 10mL volumetric flask; when the sample size is 50mg ~ 100mg Transfer the digested solution to a 25 mL volumetric flask. A.3.1.2.2 Non-silicon materials such as plastics and polymers The sample is crushed or shredded with a cryogenic pulverizer (A.2.4) to no more than 1mm x 1mm x 1mm and weighed 30mg~100mg The broken sample, accurate to 0.1 mg, was placed in a microwave digestion vessel. Add 8.0 mL of concentrated nitric acid to the digestion vessel filled with the test sample and blank. After the reaction of the sample and acid is complete, the digestion vessel will be Sealed and placed in a microwave digestion apparatus, warmed to (210 ± 5) °C in 20 minutes, and kept at (210 ± 5) °C for 10 minutes, let the sample cool to Less 5 minutes, then remove from microwave digestion apparatus. Before opening the digestion vessel, cool the digestion tank to room temperature or at least 30min. Transfer the digested solution to a suitable volumetric flask (5.5) according to the size of the sample. Rinse the digestion vessel with a small amount of water and combine. Eluent in a volumetric flask, make up to volume with water, mix, pass the aqueous phase filter (5.7), this liquid is used for ICP-AES analysis or other suitable Instrument (5.1) Analysis and Determination (6.2). A.3.1.2.3 Crystals, glass and other siliceous materials The sample was crushed with a cryogenic mill (A.2.4). Weigh 30mg ~ 100mg crushed sample, accurate to 0.1mg, placed in the microwave Solution container. Add 3 mL of concentrated nitric acid (4.1) and 1 mL of hydrofluoric acid (4.4) to the digestion vessel filled with the test sample and blank, until the sample and acid After the reaction is complete, the digestion vessel is sealed and placed in a microwave digestion apparatus. The temperature is raised to (175±5)° C. over 5.5 min and at (175±5° C.). Hold for 9.5 min, allow sample to cool for at least 5 min, then remove from microwave digestion apparatus. Before opening the digestion vessel, it should be in the fume hood The microwave digestion tank was cooled to room temperature or cooled for at least 30 minutes. Transfer the digested solution to a suitable volumetric flask (5.5) according to the size of the sample. Rinse the digestion vessel with a small amount of water and combine. Eluent in a volumetric flask, make up to volume with water, mix, pass the aqueous phase filter (5.7), this liquid is used for ICP-AES or other suitable instrument (5.1) Analysis and Determination (6.2).

Appendix B

(Informative Appendix) ICP spectrometer operating conditions Table B.1 Working Conditions of ICP Spectrometer Spectrometer Model IRIS HR IRIS Advantage ICAP JY238 JY70P JY381 P-4010 Baird PS4 ICP-2000 high frequency power generator Incident power/W 1150 1150 1000 1480 1000 1000 1150 1800 Reflection power/W - - < 5 - - < 5 < 5 < 3 Operating frequency/MHz 27.12 27.12 40.68 56 40.68 27.12 40.68 40.68 Gas line system Observational height/mm 15 15 15 18 16 13 10 15 Cooling gas/(L/min) 14 14 15 15 16 11 12 12 Auxiliary gas/(L/min) 0.5 0.5 - 1.0 1.0 1.0 1.0 0.4 Carrier gas/(L/min) - - 0.3 1.0 0.7 0.6 0.5 0.4 Nebulizer pressure/kPa (psi) 270.3 (30.06) 165.9 (24.06) - - - - - - Peristaltic pump speed/(r/min) 100 100 - - - - - - data deal with system Short wave partial integration time /s 30 10 Long wave partial integration time/s 10 5 Points 3 3 Visual element And given Visual element And given Table B.2 Elemental Analysis Wavelengths and Diffraction Levels Pb Cd Wavelength (diffraction level) 220.3 261.4 214.4 226.5 228.8 ......

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