提出了高效液相色谱法(HPLC)测定橡胶初加工废水中二硫化四甲基秋兰姆(TMTD)含量的方法。取0.1 mL胶清废水样品,用甲醇6 mL超声提取5 min,冷却至室温,用甲醇定容至10 mL。上清液经0.22 μm有机系滤膜过滤后,以Agilent ZORBAX SB-C₁₈色谱柱为固定相,40%(体积分数)甲醇溶液为流动相进行等度洗脱,采用HPLC测定其中TMTD的含量。结果表明,TMTD标准曲线的线性范围为0.50~10.00 mg·L^-1,检出限(3S/N)为0.254 mg·L^-1。对同一样品测定6次,测定值的相对标准偏差小于2.0%。对实际样品进行加标回收试验,回收率为91.4%~99.7%。

A method for the determination of tetramethylthiuram disulfide (TMTD) in rubber primary processing wastewater by high performance liquid chromatography (HPLC) was proposed. 0.1 mL of colloidal wastewater sample was taken, and extracted ultrasonically in 6 mL of methanol for 5 min. Cooling to room temperature, its volume was made up to 10 mL with methanol. The supernatant was filtered by 0.22 μm organic filter membrane, and TMTD in the above solution was determined by HPLC, using Agilent ZORBAX SB-C₁₈ column as the stationary phase and 40% (volume fraction) methanol solution as the mobile phase for isocratic elution. As shown by the results, the linear range of TMTD standard curve was 0.50-10.00 mg·L^-1, with detection limit (3S/N) of 0.254 mg·L^-1. The same sample was determined 6 times, with RSDs of the determined values less than 2.0%. The spiking recovery test was carried out on the actual sample, giving results in the range of 91.4%-99.7%.