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GB/T 28728-2012: Determination of the microstructure of solution-polymerized SBR
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GB/T 28728-2012: Determination of the microstructure of solution-polymerized SBR

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Determination of the microstructure of solution-polymerized SBR ICS 83.060 G40 National Standards of People's Republic of China Solution polymerization styrene - butadiene rubber (SSBR with) Determination of microstructure (ISO 21561.2005, Styrene-butadienerubber (SBR) -Determinationofthe microstructureofsolution-polymerizedSBR, IDT) Issued on. 2012-06-27 2013-02-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released

Foreword

This standard was drafted in accordance with GB/T 1.1-2009 given rules. This standard uses the translation method identical with ISO 21561.2005 "styrene - butadiene rubber (SBR) solution polymerization styrene - butadiene Determination rubber (SBR) microscopic structure "(in English) and amendments thereto ISO 21561.2005/Amd.1.2010 (in English). Correspondence between the consistency of the standards of international documents and normative references of the following documents. Determination of matter (ISO 1407.1992, MOD) --- GB/T 3516-2006 rubber solvent extraction; --- GB/T 15340-2008 natural and synthetic rubber raw sampling and sample preparation method (ISO 1795.2000, IDT). For ease of use, this standard made the following editorial changes. --- Modify the standard name; --- Deleted international standards foreword; --- Inclusion content of international standards amendment. The standard proposed by China Petroleum and Chemical Industry Association. This standard by the national Common test methods for rubber and rubber goods Technical Committee of Standardization Technical Committee (SAC/TC35/SC2) Centralized. This standard was drafted. China PetroChina Lanzhou Chemical Research Center, China Petroleum & Chemical Corporation North Beijing North Branch of the Academy of Yanshan, China PetroChina Dushanzi Petrochemical Research Institute, Ltd. tournament round, Beijing rubber workers Industry Research and Design Institute, Qingdao Yi Kesi New Materials Co., Ltd. The main drafters of this standard. Zhao Jialin, Wu Chunhong, Sun Feng, Wang Deyu, high Du, Bo Shaohua, Levine group Dingzhao Juan, Sun Lijun, Wang feet away, Wang Wenxiang, Wang Xiaoju, Xiejun Fang, Ding Xiaoying, Linqing Ju, Li molestation. Solution polymerization styrene - butadiene rubber (SSBR with) Determination of microstructure Warning --- personnel should use this standard regular laboratory work experience. This standard does not point out all possible security asked question. Users have the responsibility to take appropriate safety and health practices and to ensure compliance with the conditions relevant national regulations.

1 Scope

This standard specifies the use of 1H- NMR spectroscopy (jus cogens) and infrared spectroscopy (relative method) for solution polymerization SBR (SSBR) Zhong Ding Microstructure and styrene monomer content of the diene monomer was measured by quantitative analysis method. The styrene content is expressed relative to the entire The mass fraction of the polymer. 1,4-trans structure, 1,4-cis structure and a 1,2-vinyl structure content is expressed relative to the butadiene part The mole fraction. NOTE. using known microstructure content SSBRs (obtained by 1H- NMR spectroscopy) calibrated, IR must also be given microstructure Values.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document. ISO 1407 Rubber - Determination of solvent extract (Rubber-Determinationofsolventextract) ISO 1795 natural and synthetic rubber raw sampling and sample preparation method (Rubber, rawnaturalandrawsynthetic-Sampling andfurtherpreparativeprocedures) 3 nuclear magnetic resonance spectroscopy (jus cogens) 3.1 Principle 3.1.1 A small amount of extract had SSBR sample was dissolved in deuterated chloroform. 3.1.2 sample solution 1H- NMR spectra were measured at 15ppm width. Butadiene 1,4-bond (1,4-trans bond And the sum of 1,4-cis bonds) and 1,2-vinyl peak area peak area was determined together with styrene. Microstructure of butadiene and benzene The ethylene content is calculated according to the theoretical formula. 3.2 Reagents 3.2.1 deuterochloroform, CDC13 (purity > 99.8%), containing 0.03% of tetramethylsilane (TMS) as the internal standard. 3.2.2 ethanol - toluene azeotrope (ETA). 3.2.3 acetone, AR. 3.3 Instrument 3.3.1 1H- NMR spectrometer, having a frequency of 150MHz or higher Fourier transform nuclear magnetic resonance (FT-NMR). 3.3.2 extraction, such as the ISO 1407. 3.3.3 vacuum oven, operating temperature is 50 ℃ ~ 60 ℃. ...