螺口注射器自动振荡萃取法测定水中挥发酚类含量

Determination of Volatile Phenols in Water by Automatic Oscillation Extraction with Spiral Syringe

目的:运用螺口注射器代替分液漏斗检测水中挥发酚类含量。方法:通过全能振荡器代替手动振摇,对螺口注射器中的水进行定时定频振荡萃取,而后将注射器插于固相萃取装置上分离三氯甲烷相,用分光光度计比色定量。结果:在振荡器振荡强度1850 r·min^(-1)、振荡时长3 min、按照国标方法依次添加试剂的条件下,挥发酚标准曲线相关系数为0.9993,回收率为94.6%~94.9%,相对标准偏差为0.62%~3.99%,检出限为0.002 mg·L^(-1)。结论:使用螺口注射器代替分液漏斗萃取,依靠全能振荡器定时定频的特点,确保各样品萃取过程中的振荡力度和时间完全一致,固相萃取装置有效分离待测物质的同时可以大批量操作,具有快速、准确、灵敏的特点,螺口注射器还可重复利用,大大降低了检测费用。

Objective:To use a spiral shaped syringe instead of a separating funnel to detect the content of volatile phenols in water.Method:By using a universal oscillator instead of manual shaking,the water in the screw mouth syringe is extracted with a fixed time and frequency oscillation.Then,the syringe is inserted into a solidphase extraction device to separate the chloroform phase,and colorimetric quantification is performed using a spectrophotometer.Result:Under the conditions of oscillator oscillation intensity of 1850 r·min^(-1),oscillation duration of 3 minutes,and the addition of reagents according to the national standard method,the correlation coefficient of the volatile phenol standard curve was 0.9993,the recovery rate was 94.6%~94.9%,the relative standard deviation was 0.62%~3.99%,and the detection limit was 0.002 mg·L^(-1).Conclusion:Using a screw shaped syringe instead of a separating funnel for extraction,relying on the characteristic of a universal oscillator timing and frequency,ensures that the oscillation force and time during the extraction process of each sample are completely consistent.The solidphase extraction device can effectively separate the substance to be tested while operating in large quantities,with the characteristics of fast,accurate,and sensitive.The screw shaped syringe can also be reused,greatly reducing the detection cost.