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GB/T 6504-2017 English PDF (GBT6504-2017)

GB/T 6504-2017 English PDF (GBT6504-2017)

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GB/T 6504-2017: Man-made fiber -- Test method for oil content

This Standard specifies the test method for oil content of man-made fiber: extraction method (Method A), neutral soap solution washing method (Method B), optical refractive index method (Appendix A), nuclear magnetic resonance method (Appendix B), rapid extrusion method (Appendix C). This Standard is applicable to polyester (dacron), polyamide (chinlon), polyacrylonitrile (acrylic), polypropylene (polypropylene), polyvinyl formal (vinylon), regenerated cellulose fiber (rayon); other type of man-made fibers can refer to.
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 59.060.20 W 50
GB/T 6504-2017
Replacing GB/T 6504-2008
Man-Made Fiber ?€? Test Method for Oil Content
Issued on. December 29, 2017 Implemented on. July 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of PRC. Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative References ... 5
3 Terms and Definitions ... 6
4 Sampling Rules ... 6
5 Test Methods ... 6
6 Test Report ... 12
Appendix A (Normative) Optical Refractive Index Method ... 13
Appendix B (Normative) Nuclear and Magnetic Resonance Method ... 17
Appendix C (Normative) Rapid Extrusion Method ... 19
Foreword
This Standard was drafted as per the rules specified in GB/T 1.1-2009.
This Standard replaced GB/T 6504-2008 Testing Method for Oil Content of Man-Made Fibers; compared with GB/T 6504-2008, this Standard has the major technical changes as follows. ---Confirm the cellulose fibers in the scope to be regenerated cellulose fibers (rayon); add the description that can be referred to by other types of man-made fibers (see Clause 1 of this Edition; Clause 1 of Edition 2008); ---Confirm the volume of distillation flask to be 150mL in Method A of extraction method (see 5.1.4 of this Edition; 5.1.3 of Edition 2008); --- No longer measure the moisture content of the fiber in Method A of extraction method; but calculate the oil content directly through weighing the mass of dry fiber after extracting (see 5.1.6 of this Edition; 5.1.5 of Edition 2008); --- Specially propose that the Method B of soaping method is not applicable to the chinlon 6 filament, spandex filament (see 5.2.1 of this Edition; 5.2.1 of Edition 2008); --- Add Appendix C rapid extrusion method.
This Standard was proposed by China National Textile and Apparel Council. This Standard shall be under the jurisdiction of Shanghai Textile Industry Institute of Technical Supervision. Drafting organizations of this Standard. Sinopec Yizheng Chemical Fiber Company Limited, Shanghai Textile Industry Institute of Technical Supervision, Jiangyin Fibers Testing Institute, Shanghai Textile Group Testing Standard Co., Ltd., Guangdong Xinhui Meida Nylon Co., Ltd., Rongsehng Petrochemical Co., Ltd., Xin Feng Ming Group Co., Ltd., Suzhou Longjie Special Fiber Co., Ltd., Yiwu Huading Nylon Co., Ltd., Zhejiang Hengyi High-Tech Materials Co., Ltd., Tongkun Group Zhejiang Hengtong Chemical Fiber Co., Ltd., Haiyan Haili Environmental Protection Fiber Co., Ltd., Zhejiang Fiberglass New Materials Co., Ltd., Shenma Industry Co., Ltd., Shanghai Huafon Microfiber Co., Ltd., Friends of Tangshan Group Xingda Chemical Fiber Co., Ltd., Inner Mongolia Shuangxin Environment-Friendly Material Co., Ltd., Shandong Yinying Chemical Fiber Co., Ltd., Weihai Durri Synthetic Fiber Co., Ltd., China Chemical Fibers Association, and Hangzhou Best Chemical Fiber Co., Ltd. Chief drafting staffs of this Standard. He Rong, Gong Liuliu, Li Hongjie, Lu Yongliang, Luo Wenting, Shi Yujun, Guo Chengyue, Ji Wenyi, Guan Le, Zhang Shouyun, Li Qiang, Man-Made Fiber ?€? Test Method for Oil Content
Warnings. people using this Standard shall have practical working experience in the regular laboratory. This Standard doesn?€?t address all the possible safety issues. It?€?s the user?€?s responsibility to take appropriate safety and health measure and to ensure compliance with the conditions stipulated by relevant national laws and regulations. When using the solvents specified in this Standard, the Material Safety Data Sheet (MSDS) shall be read carefully. 1 Scope
This Standard specifies the test method for oil content of man-made fiber. extraction method (Method A), neutral soap solution washing method (Method B), optical refractive index method (Appendix A), nuclear magnetic resonance method (Appendix B), rapid extrusion method (Appendix C). This Standard is applicable to polyester (dacron), polyamide (chinlon), polyacrylonitrile (acrylic), polypropylene (polypropylene), polyvinyl formal (vinylon), regenerated cellulose fiber (rayon); other type of man-made fibers can refer to. 2 Normative References
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this document. GB/T 3291.1 Textiles ?€? Terms of Textile Material Properties and Test ?€? Part 1. Fiber and Yarn GB/T 3291.3 Textiles ?€? Terms of Textile Material Properties and Test ?€? Part 3. General GB/T 3921 Textiles ?€? Tests for Color Fastness ?€? Color Fastness to Washing with Soap or Soap and Soda GB/T 4146 (all parts) Textiles ?€? Man-Made Fibers
GB/T 6502 Sampling Method of Man-Made Filament Yarns
5.1.3 Reagents and materials
The reagents and materials used in this method are as follows. --- Ether. analytically pure; NOTE. if the ether is not suitable, the relevant solvent can be agreed upon by related parties. --- Qualitative filter paper. free of fat. 5.1.4 Apparatus
The apparatus used in this method is as follows. --- Fat extractor. condenser tube with height (h) of 240mm, withdrawal cylinder with diameter (d) of 37mm, length (l) of 80mm, distillation flask with volume of 150mL; --- Oven. maintain the temperature of (105??3) ??C; --- Balance. one set with minimum division value of 0.1mg and 0.01g, individually; --- Constant temperature water bath. room temperature to 100 ??C; --- Weighing container; --- Stainless steel tweezers; --- Dryer. 5.1.5 Specimen preparation
Take 2 specimens, take about 5g of staple fiber for each specimen, accurate to 0.01g; the filaments are wound together to ensure that each package is taken and evenly cut. take about 7g of pre-oriented yarns and draw yarns, accurate to 0.01g; take about 4g of textured yarn, accurate to 0.01g. 5.1.6 Test procedures
5.1.6.1 Perform the following operations continuously and repeatedly against the distillation flask at (105??3) ??C, such as drying, cooling off, weighing till the constant mass (i.e. the twice weighing difference doesn?€?t exceed 0.05% of the latter weighing), the latter weighing shall be regarded as the final mass; record the drying mass of distillation flask before extraction of m1, accurate to 0.1mg. 5.1.6.2 Pack the specimen prepared as per 5.1.4 by the qualitative filter paper into cylindrical shape; place it into the withdrawal cylinder of a fat extractor (cylinder height shall not exceed the maximum height of siphon pipe); connect the distillation flask with the known drying mass to the lower part; inject solvent 1.5 times of volume of the Appendix A
(Normative)
Optical Refractive Index Method
A.1 Scope
This method is applicable to the determination of oil content for polyester (dacron) staple fiber. A.2 Principle
Use the determination of total reflection critical angle to measure the refractive index of an unknown substance; quantitatively analyze certain compositions in the solution and check the purity of the substance. A.3 Reagents and materials
The reagents used by this method include.
--- Ether (analytically pure), methanol (analytically pure), or other reagents; --- Qualitative filter paper. free of fat;
--- Level-III water for laboratory.
A.4 Apparatus
The apparatus used in this method includes.
--- Refractive index meter. equipped with sodium light;
---Fat extractor. condense tube height (h) of 240mm, withdrawable cylinder diameter (d) of 37mm, length (l) of 80mm, distillation flask volume of 150mL; --- Oven. can maintain the temperature of (105??3) ??C; --- Balance. the minimum division value of 0.1mg; --- Constant temperature water bath. room temperature ~ 100??C; ---Measuring cylinder, pipette, stainless steel tweezers, stainless steel wire (d 2.5mm ?? l 150mm) with one end equipped with rubber tube
--- Weighing container, qualitative filter paper free of fat, mirror paper, dryer. Appendix B
(Normative)
Nuclear and Magnetic Resonance Method
B.1 Scope
This method is applicable to the determination of oil content for polyester (dacron), polyamide (chinlon), polyacrylonitrile (acrylic), polypropylene (polypropylene), polyvinyl formal (vinylon), regenerated cellulose fiber (rayon); other types of man-made fibers can refer to. B.2 Principle
Use nuclear magnetic resonance spectroscopy (NMR) to emit the pulsed magnetic field to the fiber sample; when magnetic field is canceled, inspect the response magnetic signal of the specimen; since the signal emitted by the fiber attenuates quicker than the signal emitted fiber oiling agent, the oil content of the specimen can be calculated as per the above difference. B.3 Apparatus
The apparatus used in this method includes. --- Nuclear magnetic resonance spectrometer. equipped with permanent magnets, automatic temperature control; --- Balance. minimum division value of 0.1g. B.4 Specimen preparation
Randomly and evenly take the specimen mass of 1g~5g, accurate to 0.1g.
B.5 Test procedures
B.5.1 Drawing of working curve
B.5.1.1 Take 5 specimens according to the target oil-pick-up of the product; the oil content shall be able to cover all possible range of changes; the distribution shall be as uniform as possible; it can also refer to Table B.1 for confirmation; the range can also be adjusted as per the actual oil-pick-up conditions. C.4.4 Ear washing bulb.
C.4.5 Pipette. 15mL.
C.4.6 Dryer.
C.5 Specimen preparation
Randomly and evenly take about 2g of specimen, its mass is m1, accurate to 0.1mg. C.6 Test procedures
C.6.1 Use tweezers to place the specimen into the fat lifting cylinder of the fiber fat extractor; pressurize it slightly with pressure bar. C.6.2 Place the evaporating dish (mass of m2, accurate to 0.1mg) that has been cleaned, dried to constant weight (the twice weighing difference shall not exceed 0.05% of the latter weighing), cooled off to the room temperature onto the heating loop of the fiber fat quick extractor, and fix it; the temperature of heating table is higher than the boiling point of the solvent. C.6.3 Pipette about 15mL (based on immersing the specimen) of methanol into the fat lifting cylinder of the fiber fat extractor; press the cap, which plays the role of stopping flowing; immerse for 10min. C.6.4 Remove the cap, the solvent in the fat lifting cylinder slowly drops into the evaporating dish; pay attention to prevent the overflowing, splashing, and excessive boiling of the liquid. C.6.5 When there is no solution in the oil lifting cylinder leaking, place the pressure bar into the oil lifting cylinder; squeeze till there is no liquid flowing out. C.6.6 Use tweezers to flip the squeezed specimen, loosen it; then pipette about 10mL (based on immersing the fiber) of methanol; then repeat the procedures C.6.3~C.6.5. C.6.7 After the evaporation of the second extracting solution is complete, continuously heat the evaporating dish for 10min. After that, place into the dryer to cool off to the room temperature; weigh its mass of m3, accurate to 0.1mg. C.7 Result calculation
The oil content of specimen shall be calculated by formula (C.1).

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