Citation: ZHANG Wen-Hao, LAN Ying-Jia, LU Cheng-Hua, SUN Zi-Yuan, LU Huan-Jun, LI Xiao-Hong, TU Ying-Feng. Application of Nuclear Magnetic Resonance Technology in Component Analysis of Blooming on Rubber Product Surface[J]. Chinese Journal of Analytical Chemistry, ;2023, 51(3): 405-411. doi: 10.19756/j.issn.0253-3820.221376 shu

Application of Nuclear Magnetic Resonance Technology in Component Analysis of Blooming on Rubber Product Surface

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College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, China;
2.
Su Zhou Hua Dong Rubber Industrial CO., Ltd., Suzhou 215000, China;
3.
Jiangsu Key Laboratory for Micro and Nano Heat Fluid Flow Technology and Energy Application, School of Physical Science and Technology, Suzhou University of Science and Technology, Suzhou 215009, China

Corresponding author: LI Xiao-Hong, TU Ying-Feng,
Received Date: 6 July 2022
Revised Date: 9 February 2023

Fund Project: Supported by the National Natural Science Foundation of China (No. 22071167).

Scanning electron microscopy (SEM) coupled with energy spectrometry (EDS), quantitative proton nuclear magnetic resonance (¹H NMR) and two-dimensional diffusion-ordered spectroscopy (DOSY) techniques were applied to analyze the composition of blooming. The EDS results indicated that the elements in the blooming were carbon, oxygen, sulfur and zinc with the mass ratio of 6∶1∶1∶1. Quantitative ¹H NMR combined with DOSY strongly convinced that the main precipitates of the blooming were zinc stearate, zinc dimethyl dithiocarbamate (ZDMC), 2-mercaptobenzothiazole (MBT) and rubber protective wax. Their corresponding mass content ratio was 38.9% : 31.5% : 14.4% : 15.2%, based on which the content ratio of element C, O, S and Zn was estimated as 5.70 ∶0.44 ∶1.28∶1. Then the possible formation mechanism of blooming was proposed. ZnO reacted with S to form ZnS, followed by the reaction of ZnS and stearic acid to generate zinc stearate. Moreover, tetramethyl thiuram disulfide (TMTD) could react with ZnO to produce ZDMC during the vulcanization stage. The DOSY and quantitative ¹H NMR spectroscopy were used together for the first time to analyze the components of blooming mixture on the surface of rubber products, which opened a new avenue to analyze unknown mixtures.
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沈阳化工大学材料科学与工程学院沈阳 110142