Determination of 6 Rubber Additives in Rubber by UPLC
摘 要
取条状橡胶样品(厚约2 mm,宽约1 mm)1.000 g,加入体积比为6:1的乙腈-二氯甲烷混合溶液50 mL,超声提取60 min,所得溶液经0.45 μm滤膜过滤,滤液用于超高效液相色谱法分析。用ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×100 mm,1.8 μm)为固定相,以体积比为40:60的乙腈-pH 4.0的12.5 mmol·L-1磷酸二氢钠混合溶液为流动相进行等度洗脱,使所测定的6种橡胶助剂得以分离,对6种橡胶助剂在不同波长处进行紫外检测,防老剂6PPD[N-(1,3-二甲基)丁基-N'-苯基对苯二胺]的检测波长为290 nm,防焦剂CTP (N-环己基硫代邻苯二甲酰亚胺)和其他4种硫化促进剂[TBBS (N-叔丁基-2-苯并噻唑次磺酰胺)、MBTS (2,2-二硫化二苯并噻唑)、CBS (N-环己基-2-苯并噻唑次磺酰胺)、DCBS (N,N-二环己基-2-苯并噻唑次磺酰胺)]的检测波长均为226 nm。6种橡胶助剂的标准曲线的线性范围均为5.0~500.0 mg·L-1,其检出限(3S/N)为0.3~2.5 mg·L-1。按标准加入法进行回收试验,测得回收率为82.8%~107%,测定值的相对标准偏差(n=5)均小于5.0%。
Abstract
Rubber sample strips (thickness:ca. 2 mm, width:ca. 1 mm) of 1.000 g were taken and extracted ultrasonically with 50 mL of a mixed solution of CH3CN and CH2Cl2 with the volume ratio of 6:1 for 60 min. The solution was filtered through 0.45 μm filtering membrane and the filtrate was used for UPLC analysis. ZORBAX Eclipse XDB-C18 column (4.6 mm×100 mm, 1.8 μm) was used as stationary phase, and a mixed solution of CH3CN and 12.5 mmol·L-1 NaH2PO4 (pH 4.0) with the volume ratio of 40:60 was used as mobile phase in isogradient elution, in the course of which the 6 rubber additives[i.e., the anti-aging agent 6PPD (N-(1,3-dimethylbuty)-N'-phenyl-phenylenediamine), the anti-charring agnet CTP (N-cyclohexylthiophthalimide) and 4 vulcanizing agents TBBS (N-tert-butyl-2-benzothiazole), MBTS (2,2-dibenzothiazole disulfide), CBS (N-cyclohexyl-2-benzothiazole sulfenamide) and DCBS (N,N-dicyclohexyl-2-benzothiazole sulfenamide)] were separated and their absorbances measured spectrophotometrically at different wavelengths of 290 nm (for 6PPD) and of 226 nm (for the remainder). Linearity ranges of the standard curves of the 6 rubber additives were found same between 5.0 mg·L-1 and 500.0 mg·L-1; their detection limits (3S/N) were found in the range of 0.3-2.5 mg·L-1. Test for recovery was made by standard addition method, giving recoveries ranged from 82.8% to 107%. Values of RSDs (n=5) were found all less than 5.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202001011
所属栏目 工作简报
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收稿日期 2019/5/24
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备注高明,工程师,硕士,主要从事橡胶材料测试技术管理、实验室质量管理工作,gaomingnihao1981@163.com
引用该论文: GAO Ming,XU Yanlin,SHENG Xiang,PEI Chao. Determination of 6 Rubber Additives in Rubber by UPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(1): 66~70
高明,徐艳林,盛翔,裴超. 超高效液相色谱法测定橡胶中6种橡胶助剂的含量[J]. 理化检验-化学分册, 2020, 56(1): 66~70
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参考文献
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