Page 90 - 理化检验-化学分册2025年第三期

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Determination of Sulfur in Natural Rubber by Wavelength Dispersive

X-Ray Fluorescence Spectrometry

ZHANG Zhang , DING Youchao , WU Jing , ZHANG Yue , ZHANG Tong , SUN Tingting , YAN Wenxun 1*
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(1. Nanjing Customs District Industrial Products Inspection Center, Nanjing 210019, China;
2. Jiangsu Textiles Quality Service Inspection Testing Institute, Nanjing 210007, China)
Abstract: In response to the complex and time-consuming process of existing methods for determination of sulfur in rubber,
as well as the lack of certified reference materials for natural rubber matrices currently available on the market, artificial reference
samples of natural rubber matrices with different sulfur content gradients were prepared using sulfur, zinc oxide, stearic acid,
vulcanization accelerator N-tert-butyl-2-benzothiazole sulfonamide (TBBS), and crude rubber as raw materials through artificial
batching, mixing, and vulcanization pressing. Wavelength dispersive X-ray fluorescence spectrometry was used for determination
of sulfur in natural rubber to draw the calibration curve. As shown by the results, mixing for 12 min during the preparation of the
reference samples helped to achieve uniform dispersion of sulfur element. The dispersion of sulfur element and the uniformity of
the reference samples were the best when settling at 25 ℃ for 48 h. Linear relationship between the corresponding fluorescence
intensity and mass fraction of sulfur was found in the range of 1. 0%—4. 0%, with detection limit of the method of 0. 006% (mass
fraction). This method was used to determine quality control samples 10 times in parallel, and the average value obtained was
basically consistent with the theoretical value, with RSDs less than 2. 0%. Compared with ion chromatography method of the
national standard GB/T 41946—2022, the results of the two methods were basically consistent.
Keywords: wavelength dispersive X-ray fluorescence spectrometry; natural rubber; sulfur; reference sample

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