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SN/T 1690.3-2019: (New textile fiber composition analysis method. Part 3: Qualitative identification of graphene modified fiber)
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(New textile fiber composition analysis method. Part 3: Qualitative identification of graphene modified fiber)
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SN/T 1690.3-2019
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Basic data | Standard ID | SN/T 1690.3-2019 (SN/T1690.3-2019) | | Description (Translated English) | (New textile fiber composition analysis method. Part 3: Qualitative identification of graphene modified fiber) | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | W04 | | Classification of International Standard | 59.080.01 | | Word Count Estimation | 13,110 | | Date of Issue | 2019 | | Date of Implementation | 2020-07-01 | | Issuing agency(ies) | General Administration of Customs | SN/T 1690.3-2019: (New textile fiber composition analysis method. Part 3: Qualitative identification of graphene modified fiber)
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Analysis of new type textile fiber component-Part 3.
Identification ofgraphene modified fiber
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
New type of textile fiber composition analysis method Part 3.Qualitative identification of graphene modified fiber
Issued by the General Administration of Customs of the People's Republic of China
2019-12-27 release
2020-07-01 Implementation
Foreword
SN/T 1690 "New Type of Textile Fiber Composition Analysis Method" is divided into 3 parts.
--Part 1.Determination of soybean protein composite fiber content by nitric acid method;
--Part 2.PTT, PBT fiber nuclear magnetic resonance spectroscopy;
--Part 3.Qualitative identification of graphene modified fibers.
This part is part 3 of SN/T 1690.
This part was drafted in accordance with the rules given in GB/T 1.1-2009.
This part is proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organizations of this section. Chengdu Customs of the People’s Republic of China, Jinan Shengquan Group Co., Ltd., South of the People’s Republic of China
Chang Customs, Jihua 3509 Textile Co., Ltd.
The main drafters of this section. Yu Lingyun, Gou Yuan, Pang Xiaohong, Tang Diyuan, Wang Shuangcheng, Peng Guobao, Ma Junqiang, Wei Jian, Dong Wei,
Geng Xiang, Liu Fei, Wu Mengru, Guo Jie, Miao Xinyun.
New type of textile fiber composition analysis method Part 3.Qualitative identification of graphene modified fiber
1 Scope
This part of SN/T 1690 specifies the requirements of graphene-modified nylon fiber, graphene-modified viscose fiber, and graphene-modified polyester fiber.
Qualitative identification method.
This section applies to the qualitative identification of graphene-modified nylon fibers, graphene-modified viscose fibers and graphene-modified polyester fibers.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version is applicable to this
file. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
FZ/T 01057.1 Textile Chemical Fiber Part 1.General Instructions
3 Terms and definitions
The following terms and definitions apply to this document.
3.1 Graphene graphene
Each carbon atom is SP2 hybridized with three adjacent carbon atoms to form a honeycomb structure of carbon atom layer.
[T/CGIA 001-2018, definition 2.1]
3.2 Graphene modified fiber
Take other materials as basic raw materials, add graphene, and prepare fiber structure features and graphene functions through different spinning processes
Sex as one fiber.
[T/CGIA 002-2018, definition 3.3]
3.3 Graphene nylon fiber
Using polyamide as the basic raw material, through the graphene blending melt spinning process, the nylon fiber structure characteristics and graphene function are prepared.
A fiber that integrates performance.
[T/CCFA 01034-2017, definition 3.1]
3.4 Graphene viscose fiber
Graphene is blended with cellulose fiber pulp as the basic raw material, and the wet spinning process is used to prepare viscose staple fiber structure.
It is a fiber that combines the functional properties of graphene.
[T/CCFA 01032-2017, definition 3.1]
3.5 Graphene polyester fiber
Using polyester (PET) as the basic raw material, through the graphene blending melt spinning process, the preparation has the structural characteristics of polyester fiber and graphite
A fiber with ene functionality as a whole.
[T/CCFA 01031-2017, definition 3.1].
4 Principle
According to the different physical and chemical properties of the graphene modified fiber, different analysis methods are used, and the test results are compared with Appendix A~
Record D for qualitative analysis.
5 Sample
The sampling and preparation of the sample shall be carried out in accordance with the provisions of FZ/T 01057.1.
6 Qualitative analysis
6.1 Microscopy
6.1.1 Test instruments and tools
Hastelloy slicers, slides, coverslips, biological microscopes.
6.1.2 Reagents
Liquid paraffin.
6.1.3 Test method
6.1.3.1 Longitudinal observation
Tear the sample into thin bundles and arrange them in order, take a sample of appropriate length, place it on a glass slide, add a small amount of liquid paraffin, and cover with a cover glass
Place it on the stage of a biological microscope of 100 times to 500 times to observe its shape, and record the longitudinal characteristics of the sample.
6.1.3.2 Cross-sectional observation
Place the cross-section of the sample prepared with the Hastelloy microtome on a glass slide, add a small amount of liquid paraffin, and cover with a cover glass (be careful not to
To bring in air bubbles), place it on the stage of a biological microscope at 100 to 500 times to observe its shape, and record the cross-sectional characteristics of the sample.
6.1.4 Identification
Refer to Appendix A, and refer to Appendix C and Appendix D for identification.
6.2 Dissolution method
6.2.1 Test instruments and tools
6.2.1.1 Thermometer (0℃～100℃).
6.2.1.2 Analytical balance (sensitivity 1 mg).
6.2.1.3 Electric heating constant temperature water bath (30℃～100℃).
6.2.1.4 Electric furnace, glass suction filter bottle, beaker, test tube, tweezers, glass rod, crucible tongs.
6.2.2 Reagents
Unless otherwise specified, all reagents used are of analytical grade. The water is Grade 3 water specified in GB/T 6682.
Concentrated sulfuric acid (with a density of 1.83 g/L at 20 ℃), concentrated hydrochloric acid (with a density of 1.18 g/L at 20 ℃), concentrated nitric acid (with a density of 1.40 g/L at 20 ℃),
Formic acid (density 1.12 g/L at 20 ℃), hydrofluoric acid (density 1.15 g/L at 20 ℃), sodium hydroxide, N-dimethylformamide, dimethyl formamide
Sulfoxide, sodium hypochlorite, cyclohexanone, cuproamine, glacial acetic acid, acetone, tetrahydrofuran, potassium thiocyanate, phenol, copper cyclohexanone, acetonitrile, pyridine
Pyridine, carbon tetrachloride, dichloromethane, dioxane, ethyl acetate.
6.2.3 Test method
Put about 100 mg of sample in a test tube, and inject 10 mL of reagent (the bath ratio of sample to reagent is 1.100). At room temperature, use glass
Stir the rod for 5 minutes and observe the dissolution of the reagent on the sample. Samples that are difficult to dissolve at room temperature need to be boiled and stirred with a glass rod
Move for 3 min, depending on the degree of dissolution. Record the dissolution of the sample in various solvents and conditions.
Note 1.The test should be carried out in a fume hood, because many solvents are highly volatile and toxic; do not use open flames when heating, pay attention to fire prevention
Safe because many reagents are flammable.
Note 2.Normal temperature refers to (25-30)℃, and boiling refers to the boiling of the solvent.
6.2.4 Identification
Compare with Appendix B, and refer to Appendix C and Appendix D for identification.
6.3 Raman spectroscopy
6.3.1 Principle
When a laser beam irradiates the sample, an inelastic collision occurs between the sample molecule and the photon, that is, Raman scattering occurs. With the aid of the instrument
By plotting the intensity value of Raman scattering with the corresponding Raman shift value, the Raman spectrum of the sample can be obtained, and each characteristic peak of Raman shift in the spectrum
Both contain information about the molecular structure of the sample. Different substances have different Raman spectra. Using this principle, the unknown fiber and the known fiber
Vi's Raman spectra are compared to distinguish fiber types.
6.3.2 Instruments and tools
Raman spectrometer. with a laser light source, the wavelength of the light source is 532 nm or 785 nm, and the spectral range is not less than 300 cm-1～3500 cm-1,
The spectral resolution is better than 5 cm-1.
6.3.3 Test method
6.3.3.1 Turn on the instrument
According to the operating procedure of the instrument, turn on the Raman spectrometer, warm up for half an hour until the instrument is stable, and select 0.4 MW of power.
6.3.3.2 Choose appropriate scanning conditions
Choose the appropriate light source wavelength and scan times.
6.3.3.3 Test sample
Clamp the sample into the focus bracket of the Raman spectrometer laser, and then measure, record the Raman dispersion of 300 cm-1～3500 cm-1
Radio spectrum. The test site of the sample should cover all the fibers in the sample.
6.3.4 Identification
Refer to Appendix C and Appendix D for identification. Clarify the selected area and position of the selected area scan and the selected point scan, the peak of the graphene G peak
The peak position is near 1580 cm-1; the peak position of D peak is near 1270 cm-1～1450 cm-1; the 2D peak is near 2700 cm-1.Compare graphene
In the measurement results of the modified fiber, if the peak positions are consistent and I2D/IG ≥ 0.35, it means that the fiber contains graphene.
7 Test report
The test report should include but not limited to the following.
a) If a special pretreatment is used to remove the slurry or finishing agent, it must be explained in detail;
b) Experimental results;
c) Any other details that deviate from this section and descriptions of abnormal situations.
Appendix A
(Informative appendix)
Graphene modified fiber cross-sectional and longitudinal morphological characteristics table
Appendix B
(Normative appendix)
Graphene modified fiber chemical solubility table
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