GB/T 43314-2023Silicone rubber—Determination of phenyl and vinyl content—1H-NMR method (English PDF)
硅橡胶 苯基和乙烯基含量的测定 核磁共振氢谱法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
November 27, 2023
Implementation date
June 1, 2024
Scope
GB/T 43314-2023 is the English-translated version of 硅橡胶 苯基和乙烯基含量的测定 核磁共振氢谱法.
GB/T 43314-2023 describes how to measure the phenyl and vinyl content of silicone raw rubber by proton NMR.
The sample is dissolved in NMR-grade deuterated tetrahydrofuran of purity greater than 99.5% mole fraction, free of tetramethylsilane internal standard, and run on an FT-NMR spectrometer with a 1H resonance frequency of 400 MHz or higher, using a 5 mm quartz tube and a balance accurate to 0.1 mg; the contents follow from the chemical shifts and integrated peak areas of the phenyl, vinyl and methyl protons.
Clause 1 states that the method applies to MPVMQ and DPVMQ raw rubbers, which carry phenyl in the side chain, and to VMQ, which does not, and that it does not apply to phenylene silicone rubber.
It quotes GB/T 15340 for sampling. Issued on 27 November 2023, it has applied since 1 June 2024.
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Document preview — GB/T 43314-2023
National Standard of the People's Republic of China
- ICS
- 83.060
- Classification
- G 34
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Normative reference documents
- 3 Terms and definitions
- 4 Principles
- 5 Reagents
- 6 Instruments and equipment
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.
1 Scope
This document describes a method for the determination of phenyl and vinyl content in silicone rubber by proton nuclear magnetic resonance spectroscopy.
This document applies to monophenylmethylvinyl silicone rubber raw rubber (MPVMQ) and diphenylmethylvinyl silicone containing phenyl groups in the side chain.
Rubber raw rubber (DPVMQ) and methylvinyl silicone rubber raw rubber (VMQ) without phenyl groups in the side chain. This document does not apply to phenylene silicone rubber.
2 Normative reference documents
The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, the dated quotations For undated referenced documents, only the version corresponding to that date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to this document.
GB/T 15340 Natural and synthetic raw rubber sampling and sample preparation methods
3 Terms and definitions
There are no terms or definitions to be defined in this document.
4 Principles
Dissolve a certain amount of silicone rubber raw rubber sample in deuterated tetrahydrofuran, and measure the NMR hydrogen of the sample under specified parameter conditions.
Spectrum, obtain the peak areas of different protons in phenyl, vinyl and methyl groups. Through the chemical shift and peak integrated area of protons under different chemical environments value to determine the phenyl and vinyl content in silicone rubber.
5 Reagents
Deuterated tetrahydrofuran (C4D8O). purity greater than 99.5% (mole fraction), does not contain tetramethylsilane (TMS) internal standard, NMR grade.
6 Instruments and equipment
6.1 Fourier transform nuclear magnetic resonance spectrometer (FT-NMR). 1H resonance frequency is 400MHz or higher.
6.2 Analytical balance. accuracy is 0.1mg.
6.3 Sample tube. outer diameter is 5mm, made of quartz.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
Referenced standards
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Related Standards
GB/T 15340-1994 — Rubber, raw, natural and synthetic--Sampling and further preparative procedures
GB/T 15340-2008 — Rubber, raw natural and raw synthetic - Sampling and further preparative procedures
GB/T 15340-2025 — Rubber, raw natural and raw synthetic - Sampling and further preparative procedures
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GB/T 43314-2023
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