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
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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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