GB/T 30157-2013Textiles - Determination of the total content of lead and cadmium (English PDF)

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

China's national method for the total lead and total cadmium in textiles - the two heavy metals that reach a textile not through the fibre but through what is added to it: the pigments of a plastisol print, the stabilisers of a PVC coating, the metal trim, the zips and the badges, and that matter because the article is worn against the skin and, in the case of children's clothing, chewed. The standard specifies the method for the determination of the total lead and total cadmium content of textile products, and it applies to textile products of every kind. What distinguishes a total content determination from the extraction methods used elsewhere is the question being answered. An extraction asks how much metal would come out of the article under a simulated contact; a total content determination asks how much is there at all, and it is the figure a regulation or a purchaser's specification is normally written against, because it does not depend on the extraction conditions chosen. The sample is therefore digested completely, so that the metal is brought into solution regardless of the form in which it was bound, and the solution is then measured by atomic spectrometry against calibration solutions prepared in a matching acid matrix, with the laboratory water meeting GB/T 6682. The standard sets the preparation and homogenisation of the sample, which is where a non-uniform article such as a printed garment can produce almost any answer, the digestion procedure and the reagents, the instrumental conditions, the blank and the recovery checks, and the calculation and expression of the results. It carries the warning that the user must have practical laboratory experience and is responsible for the appropriate safety and health measures. Issued on 17 December 2013 and in force since 15 October 2014, it is held by SAC/TC 209/SC 1.

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.

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.

0.5 mL,

5.7 Aqueous filtration membrane. 0.45 µm pore size.

5.8 Balance. The accuracy is 0.01mg.

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;

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

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 <