GB/T 43314-2023 in English

VALID

Silicone rubber—Determination of phenyl and vinyl content—1H-NMR method

Issued on:2023-11-27
Implemented on:2024-06-01
File Format:PDF
Delivery:Via email within 1~3 business days

Price(USD)： $160.00
$156.00

Standard No:	GB/T 43314-2023
Document status:	VALID
Title in English:	Silicone rubber—Determination of phenyl and vinyl content—1H-NMR method
Title in Chinese:	硅橡胶　苯基和乙烯基含量的测定　核磁共振氢谱法
Language:	English
File Format:	Electronic (PDF)
Delivery:	Via email within 1~3 business days
Issued on:	2023-11-27
Implemented on:	2024-06-01
ICS Classification:	83.060-Rubber
Chinese Classification:	G34-Basic standard and general method for synthetic rubber
Professional Classification:	GB-National Standard
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《GB/T 43314-2023硅橡胶　苯基和乙烯基含量的测定　核磁共振氢谱法》由TC35（全国橡胶与橡胶制品标准化技术委员会）归口，主管部门为中国石油和化学工业联合会。

Introduction

National Standard of the People's Republic of China GB/T 43314—2023

This standard specifies the method for determining the phenyl and vinyl content in silicone rubber by hydrogen nuclear magnetic resonance spectroscopy, which is applicable to monophenylmethylvinyl silicone rubber (MPVMQ) containing phenyl groups on the side chain, diphenylmethylvinyl silicone rubber (DPVMQ) and methylvinyl silicone rubber (VMQ) without phenyl groups on the side chain. The following is a detailed interpretation of the standard:

1. Background of Standard Formulation

With the continuous expansion of the application field of silicone rubber, the performance requirements for it are increasing. The phenyl and vinyl content are important indicators that affect the performance of silicone rubber. Accurate determination of these components is of great significance for product quality control. This standard provides an accurate and efficient determination method based on the technical advantages of hydrogen nuclear magnetic resonance spectroscopy (FT-NMR).

2. Comparison of standard frameworks

Standard dimensions	Scope of application	Determination method	Precision requirements
MPVMQ	Monophenylmethylvinyl silicone rubber	NMR hydrogen spectroscopy method, phenyl content calculation formula see formula (1)	Repeatability: r ≤ 0.05; Reproducibility: R ≤ 0.1
DPVMQ	Diphenylmethylvinyl silicone rubber	NMR hydrogen spectroscopy method, phenyl content calculation formula see formula (2)	Repeatability: r ≤ 0.15; Reproducibility: R ≤ 0.3
VMQ	Methyl vinyl silicone rubber	NMR hydrogen spectroscopy, the formula for calculating the vinyl content is shown in formula (3)	Reproducibility: r ≤ 0.1; Reproducibility: R ≤ 0.25

3. Experimental Principle and Method

The experiment uses nuclear magnetic resonance hydrogen spectroscopy to calculate the content of phenyl and vinyl in silicone rubber by measuring the chemical shift and peak integrated area value of protons under different chemical environments. The following are the key steps:

Reagent requirements: Use xenon-substituted tetrahydrofuran (C4D8O) with a purity greater than 99.5% (molar fraction) without TMS internal standard.
Instrument: Equipped with a Fourier transform nuclear magnetic resonance spectrometer (FT-NMR) with a frequency of 400MHz or higher.
Sample treatment: The silicone rubber sample was dissolved in xenon-substituted tetrahydrofuran and allowed to stand for 24 hours before the measurement was completed.

4. Result calculation and precision analysis

The calculation formula for the content of phenyl and vinyl is as follows:

Example:For MPVMQ sample, the calculation formula for the molar percentage of phenyl is: $$ w_{\mathrm{p},1}=\frac{6S_{1}}{3S_{1}+5S_{2}+5S_{3}}\times100 $$

5. Implementation suggestions

To ensure the accuracy of the test results, it is recommended that:

Operate in strict accordance with the reagent and instrument requirements specified in the standard.
The laboratory should be equipped with professional personnel and the equipment should be calibrated regularly.
For complex samples, it is recommended to conduct multiple parallel tests to improve precision.

More samples: JGJ 94-2008 DL/T 5154-2012 GB 50021-2001(2009)

Sample only — not a preview of GB/T 43314-2023

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