GB/T 39113-2020 English PDF

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GB/T 39113-2020: Footwear - Critical substances potentially present in footwear and footwear components - Determination of phenol
Status: Valid

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Basic data

Standard ID: GB/T 39113-2020 (GB/T39113-2020)
Description (Translated English): Footwear - Critical substances potentially present in footwear and footwear components - Determination of phenol
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: Y78
Classification of International Standard: 61.060
Word Count Estimation: 14,132
Date of Issue: 2020-10-21
Date of Implementation: 2021-05-01
Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration

GB/T 39113-2020: Footwear - Critical substances potentially present in footwear and footwear components - Determination of phenol

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Footwear - Critical substances potentially present in footwear and footwear components - Determination of phenol ICS 61.060 Y78 National Standards of People's Republic of China Restricted substances in footwear and footwear components Determination of phenol 2020-10-21 released 2021-05-01 implementation State Administration for Market Regulation Issued by the National Standardization Management Committee

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. The translation method used in this standard is equivalent to ISO 20536.2017 ``Limited Substances Existing in Footwear and Footwear Parts in Footwear Materials Determination of Phenol. The Chinese documents that have a consistent correspondence with the international documents cited in this standard are as follows. ---GB/T 12810-1991 Laboratory glass instrument glass measuring device capacity calibration and use method (ISO 4787.1984, IDT) This standard has made the following editorial changes. ---In order to be consistent with the existing domestic footwear standard system, the standard name is changed to "Limited substances in footwear and footwear components Determination of Quality Phenol; ---Informative Appendix A adds A.4, leading to Figure A.1. Please note that certain contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents. This standard was proposed by the China National Light Industry Council. This standard is under the jurisdiction of the National Footwear Standardization Technical Committee (SAC/TC305). Drafting organizations of this standard. China Leather and Footwear Research Institute Co., Ltd., Zhejiang Aokang Footwear Co., Ltd., China Leather and Shoemakers Industry Research Institute (Jinjiang) Co., Ltd. The main drafters of this standard. Shi Yiwei, Wang Zhentao, Meng Hongwei, Wang Jinquan, Ran Meiling. Restricted substances in footwear and footwear components Determination of phenol Warning---Users of this standard should have working experience in a formal laboratory. This standard does not point out all possible safety issues. The user is responsible for taking appropriate safety and health measures.

1 Scope

This standard specifies the determination method of phenol in footwear and footwear components. This standard applies to all footwear components except metal. Note. Table 1 in ISO /T R16178.2012 gives the definition of the materials involved in this test method.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated references, the latest version (including all amendments) applies to this document. ISO 4787 Laboratory Glass Apparatus. Apparatus for use and capacity test methods for measuring volume Terms and definitions are not listed in this standard.

4 Principle

The sample was cut into small pieces, and the toluene/acetone mixed solution with a volume ratio of 80/20 was ultrasonically extracted in a closed bottle at 60℃ for 1h. The extract was analyzed by gas chromatography/mass spectrometry (GC-MS). This method uses an extraction substitute (phenol-D6), which is added before the extraction step and quantified in the same way as the target compound. extraction The surrogate is used to monitor the extraction rate and calculate the recovery rate. Anthracene-D10 was used as an internal standard and added to the sample vial (sample and calibration) before chromatographic analysis. The internal standard is used to calibrate the calibration curve.

5 Reagents and materials

5.1 Chemicals The substances mentioned in this standard should be used with limited purity. ---The purity of the product used for the standard is above 95%; ---The solvent is analytically pure. 5.1.1 Phenol CAS. 108-95-2 (target compound). 5.1.2 Phenol-D6CAS. 13127-88-3 (extraction substitute). 5.1.3 Anthracene-D10CAS. 1719-06-8 (internal standard). 5.1.4 Toluene CAS. 108-88-3 (solvent). 5.1.5 Acetone CAS. 67-64-1 (solvent). 5.1.6 A mixture of toluene/acetone with a volume ratio of 80/20 (mixed extract). The composition of the mixture is based on volume. For example, to prepare a 100mL mixture, 80mL of toluene and 20mL of acetone need to be mixed. 5.1.7 Methanol CAS. 67-56-1 (solvent). 5.2 Stock solution 5.2.1 Internal standard─anthracene-D10─stock solution (1000mg/L) Weigh 10mg of anthracene-D10 in a 10mL volumetric flask and dilute with acetone. Then transfer the prepared solution to PTFE (PTFE) stopper in a 10mL brown vial and store at 4°C. 5.2.2 Internal Standard─Anthracene-D10─Working Solution (10mg/L) Prepare stock solution (5.2.1) 1.100 dilution. For example, take 100μL of stock solution in a 10mL volumetric flask and use acetone to make the volume constant. 5.2.3 Extraction substitute——phenol-D6─stock solution (1000mg/L) Weigh 10mg of phenol-D6 in a 10mL volumetric flask and dilute with acetone. Then transfer the prepared solution to the PTFE stopper In a 10mL brown vial, and store at 4°C. 5.2.4 Extraction Substitute——Phenol-D6─Working Solution (10mg/L) Prepare stock solution (5.2.3) 1.100 dilution. For example, take 100μL of stock solution in a 10mL volumetric flask and use acetone to make the volume constant. 5.2.5 Target compound-phenol-stock solution (1000mg/L) Weigh 10mg of phenol in a 10mL volumetric flask and dilute with acetone. Then transfer the prepared solution to the one with PTFE stopper 10mL brown vial and store at 4°C. 5.2.6 Phenol Phenol-D6-Calibration Intermediate Solution (10mg/L) Take 100 μL of the extraction substitute stock solution (5.2.3) and the target compound stock solution (5.2.5) in a 10 mL volumetric flask, and use toluene/acetone (80/20) mixture is constant volume. 5.2.7 Phenol phenol-D6─calibration working solution (1mg/L) Take 1000μL of calibration intermediate solution (5.2.6) in a 10mL volumetric flask, and use a toluene/acetone (80/20) mixture to make the volume constant.

6 Instruments

Common laboratory equipment and the following equipment, as well as laboratory glassware complying with ISO 4787. 6.1 Analytical balance with an accuracy of at least 0.1mg. 6.2 Glass bottle, sealable, 40mL. 6.3 Ultrasonic water bath, temperature controllable. 6.4 PTFE membrane filter, the pore width is 0.45μm. 6.5 2mL sample bottle, PTFE cap. 6.6 20mL sample bottle, polytetrafluoroethylene cap. 6.7 Gas chromatograph equipped with a mass selective detector (MSD), or other chromatographic techniques that have been confirmed to be used for this analysis.

7 sampling

The uppers, composite linings and inner pads in shoes should be tested. The sample is composed of a single material (leather, fabric or polymer). Homogeneous fabric, leather and polymer samples are cut into pieces with different sides More than 5mm. The sample should not be ground, because grinding will cause the loss of phenol volatility.

8 Test method

8.1 Extraction Weigh 1g sample into a 20mL glass bottle (6.6). Then add 9.8mL of mixed extract (5.1.6) and.200μL of extraction Substitute working fluid (5.2.4). Ultrasonic extraction (60±2)min at (60±5)℃. Note. It has been confirmed that acetone is effective as an extraction solvent. However, its higher polarity (compared to the mixed extract) can cause a large amount of co-extraction in the extract Compounds (such as dyes or other polar compounds such as ethylene glycol), these may interfere with the analysis. Some polymeric materials will dissolve in the mixed extract and cause quantitative problems. In this case, methanol can be used for precipitation. Join 20mL methanol (5.1.7) precipitation at least 5min, if necessary, filter with a 0.45μm PTFE membrane filter. 8.2 Analysis Take 1mL of the obtained extract and add 50μL of internal standard working solution (5.2.2). According to Chapter 9, GC-MS (6.7) was used for analysis. 8.3 Calibration For practical reasons, calibration is performed with a solution containing the target compound and extraction substitute. At least 5 measuring points with different concentrations in the linear range. Calibrate directly with a 2mL sample bottle, see Table 1. 9 GC-MS determination 9.1 Measuring method In addition to the methods described in Appendix A, other analytical methods can also be used if they reach comparable accuracy and limit of quantification (9.3.1). The ions given in Table 2 should be used. Examples are given in Appendix A. 9.2 Quantitative 9.2.1 Calibration curve Use the ratio of (Ae/Ais) and (Ce/Cis) in formula (1) to establish a linear regression function. 9.2.2 Recovery rate After using the extraction substitute, the extraction rate is calculated by formula (2). If the extraction rate is lower than 75% or higher than 125%, the sample should be re-analyzed. 9.2.3 Determination of phenol content Calculate the phenol content according to formula (3), expressed as mass fraction W (mg/kg). 9.3 Measurement method performance 9.3.1 Limit of quantification of GC-MS method Taking into account the sample mass of 1g and the extraction volume of 10mL, the limit of quantification of this method should be 0.5mg/kg. The extract is concentrated to 1mL under a gentle nitrogen flow, which can reduce the limit of quantification. 9.3.2 Tests between laboratories Appendix B shows the results of the inter-laboratory test. 10 Test report The test report should include the following. a) The standard number; b) test date; c) A detailed description of the test sample; d) Type of material tested (see Chapter 7); e) If necessary, storage conditions before the test; f) The content of extracted phenol calculated according to 9.2.3; g) Any deviation from this standard.

Appendix A

(Informative appendix) Example of equipment test method A.1 General Through a gas chromatography/mass spectrometer equipped with a single quadrupole/MS, phenol and phenol-D6 were analyzed in SIM/SCAN synchronous mode. A.2 Chromatographic conditions Chromatographic column. DB-5MS (or equivalent to 5% phenyl-95% dimethyl polysiloxane). Size. 30m×0.25mm×0.25μm. Carrier gas. helium gas with a linear flow rate of 36 cm/s. Column thermostat. Keep at 50°C for 1 min. Increase to 245°C at 15°C/min. Increase to 300°C at 25°C/min within 4 minutes. Sampler. Inject a volume of 1μL at 265℃ in pulsed splitless mode. Pulse pressure. 120kPa within 1.5min. Split. 60mL/min at 1.5min. Note. In order to better separate toluene and phenol, a more polar column can be used, such as DB-35 (35% phenyl), VF-17 (50% phenyl) or DB-WAX (100% polyethylene glycol). A.3 Test conditions Transmission line. 280℃. Single quadrupole MS operating in SIM/SCAN mode synchronization. The mass scanning range is between 50m/z and 300m/z. The ions focused in SIM mode are shown in Table 2. A.4 Example According to the above chromatographic conditions and detection conditions, the total ion chromatogram of phenol and internal standard standard solution (500μg/L) is shown in Figure A.1. ......

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