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GB/T 46325-2025: Vulcanized rubber - Determination of free sulfer content - Gas chromatography (GC) method and high performance liquid chromatography(HPLC)method
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GB/T 46325-2025: Vulcanized rubber - Determination of free sulfer content - Gas chromatography (GC) method and high performance liquid chromatography(HPLC)method

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ICS 83.060 CCSG40 National Standards of the People's Republic of China Determination of free sulfur content in vulcanized rubber by gas chromatography Spectroscopic methods (GC) and high-performance liquid chromatography (HPLC) Published on 2025-10-05 Implemented on May 1, 2026 State Administration for Market Regulation The State Administration for Standardization issued a statement.

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1.Structure and Drafting Rules of Standardization Documents". Drafting. This document is modified to adopt ISO.2016 3.2019 "Gas chromatography (GC) and high performance liquid chromatography (HPLC) for the determination of free free corrosive organic compounds in vulcanized rubber". Sulfur content. This document has undergone significant structural changes compared to ISO.2016 3.2019.A table comparing the structural numbering changes between the two documents is provided. See Appendix A. The technical differences between this document and ISO.2016 3.2019, and the reasons therefor, are as follows. ---Added Method C (Liquid-phase non-derivative method) and its corresponding testing principle, instruments and reagents used, testing procedures, and result description. The method for preparing standard solutions is described above because it is simpler to operate and has lower toxicity than methods A and B (see Chapters 4-10, Appendix). Record D); ---The purity type of ammonium acetate in section 6.10 has been changed from "analytical grade" to "chromatographic grade" to obtain better test results; ---The sample preparation steps for Methods A and B in Chapter 8 have been modified, adding requirements for sample particle size and recommending extraction solvents. The extraction time was adjusted, the amount of diluent and the volumetric flask volume were changed, and a blank test was added to facilitate operation and test results. precise; ---The split ratio for gas chromatography-MS in section 9.1 has been changed from "42" to "10.1" to facilitate the testing of target compounds; ---The calculation formulas for Method A and Method B in section 10.2 have been modified to include the blank test concentration in the formulas. The following editorial changes have also been made to this document. ---The units of measurement for free sulfur content in Method A and Method B have been modified (see Chapters 10 and 12). ---The errors in the international standard formula have been improved and corrected. Please note that some content in this document may involve patents. The issuing organization of this document assumes no responsibility for identifying patents. This document was proposed by the China Petroleum and Chemical Industry Federation. This document is under the jurisdiction of the General Test Methods Subcommittee of the National Technical Committee on Standardization of Rubber and Rubber Products (SAC/TC35/SC2). This document was drafted by. Guizhou Tyre Co., Ltd., Northwest Rubber & Plastics Research & Design Institute Co., Ltd., and Zhongce Rubber Group Co., Ltd. Limited Liability Company, Shandong Huasheng Rubber Co., Ltd., Guangzhou Synthetic Materials Research Institute Co., Ltd., Shandong Linglong Tire Co., Ltd., Triangle Wheel Tire Co., Ltd., Wanli Tire Co., Ltd., Sailun Group Co., Ltd., Fengshen Tire Co., Ltd., Xi'an New Ideas Rubber & Plastics Materials Co., Ltd., Shandong Yanggu Huatai Chemical Co., Ltd., Liaocheng Jingge Synthetic Materials Co., Ltd., Zhuzhou Times New Materials Technology Co., Ltd. Technology Co., Ltd., Jiangsu Qixiang High-Tech Materials Co., Ltd., Bayi Rubber Co., Ltd., Double Coin Group Shanghai Tire Research Institute Co., Ltd. The company, Beijing Academy of Science and Technology Analysis and Testing Institute (Beijing Physical and Chemical Analysis and Testing Center), and Beijing Rubber Industry Research and Design Institute have Limited Liability Company, Beijing Rubber & Tire Testing Technology Service Co., Ltd. The main drafters of this document are. Pi Chengyan, Feng Ping, Teng Xiaoxiao, Liu Yaoxin, Li Jian, Zuo Lili, Zhang Yuliang, Xu Kai, Peng Jun, Zhu Jiajun, and Liu Li. Lu Bo, Li Wei, Yan Wenli, Han Xiao, Yu Han, Huang Yanjun, Zheng Ningjuan, Ge Yongliang, Jia Yuanshan, Fang Zhao, Zhu Jinwei, Huang Cunying, Liu Xiuzheng, Liu Wanxing Shen Tanxiao, Huang Anmin, Yao Xiang, Peng Hualong, Yang Shuo, Yao Ming, Dong Wenwu, Shao Peng, Zhou Yang, Ding Xiaoying, Wang Na, Niu Danwei, Luo Lingxi. Determination of free sulfur content in vulcanized rubber by gas chromatography Spectroscopic methods (GC) and high-performance liquid chromatography (HPLC) Warning 1.Users of this document should have practical experience working in a formal laboratory. This document does not cover all possible safety hazards. Users are responsible for taking appropriate safety and health measures and ensuring compliance with relevant national regulations. Warning 2---Some steps outlined in this document may involve the use or generation of certain wastes, which may pose a hazard to the local environment. The relevant documents should specify appropriate safe operating procedures and post-use disposal of waste.

1 Scope

This document describes a method for determining the content of unconsumed inorganic free sulfur (Sx) during rubber vulcanization using chromatography. This method primarily... Used to compare the free sulfur content in rubbers with different degrees of vulcanization. Note 1.In this document, "inorganic free sulfur" is replaced with "free sulfur". Note 2.The free sulfur content determined by this method does not include sulfur in the vulcanizing agent.

2 Normative references

The contents of the following documents, through normative references within the text, constitute essential provisions of this document. Dated citations are not included. For references to documents, only the version corresponding to that date applies to this document; for undated references, the latest version (including all amendments) applies. This document. GB/T 3516-2024 Determination of solvent extractables in rubber (ISO 1407.2023, IDT)

3 Terms and Definitions

This document does not contain any terms or definitions that need to be defined. 4.Principles Free sulfur can be quantitatively analyzed using the following three methods. gas chromatography-mass spectrometry (GC/MS) or gas chromatography-flame ionization. Chemical detection method (GC/FID) (Method A), high performance liquid chromatography derivatization method (HPLC/UV) (Method B), and high performance liquid chromatography non-derivatization method Method (HPLC/UV) (Method C). For vulcanized rubber samples from methods A and B, extraction was first performed according to method B in GB/T 3516-2024.Pre-extracted solvent was then added to the resulting solution. Known amounts of triphenylphosphine (TPP). TPP reacts with free sulfur to form the stable compound triphenylphosphine sulfide (TPPS), derivatization reaction equation. The formula is shown in Figure 1. TPPS compounds contain aromatic rings and have the following advantages. First, it has more active chromophores than free sulfur, and is therefore easier to detect in HPLC/UV; ---Secondly, it has sufficient thermal stability to be injected into the GC. The following quantitative methods are applicable to both GC and HPLC chromatography. The sample used in GC (Method A) and HPLC derivatization methods (Method B) is... The preparation methods are the same. ---When the free sulfur content in the sample is unknown, the standard addition method is preferred, as this method can correct for matrix effects. ...