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A simple and rapid method for determination of petroleum oils in sewage sludge samples with ultrasonic solvent extraction by infrared spectrophotometry under optimized analytical conditions

机译:在优化分析条件下用超声波分光光度法萃取超声波溶剂萃取测定污泥样品中石油的简便快捷方法

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摘要

This study presents an analytical method for the determination of petroleum oils in sewage sludge samples using infrared spectrophotometry. The proposed method is based on the use of ultrasonic solvent extraction for sample preparation. Analytical conditions were studied and optimized through uniform experimental design of U9*(9~5). The optimized experimental conditions were obtained as follows: the extraction temperature was 50 °C, the extraction time was 45 min, the volume of extractant was 30 mL, and the ultrasonic power was at 250 W. The moisture content of the sewage sludge samples was below 10%. Similar extraction effects could be achieved through both ultrasonic solvent extraction and Soxhlet extraction methods. The detection limit was 0.9 mg kg~(-1) (k = 3, N= 8) with 91.6-102.0% recovery. The relative standard deviation (RSD, n = 5) for the measurements of the sewage sludge samples was in the range of 1.6% and 3.5%. The proposed method was validated by the analysis of simulation soil samples and successfully applied to the determination of petroleum oils in real samples of sewage sludge with satisfactory results.
机译:这项研究提出了一种使用红外分光光度法测定污水污泥样品中的石油的分析方法。所提出的方法是基于使用超声溶剂萃取进行样品制备的。通过统一的U9 *(9〜5)实验设计研究和优化了分析条件。得到了优化的实验条件,提取温度为50℃,提取时间为45min,提取液体积为30mL,超声功率为250W。低于10%。通过超声溶剂萃取和索氏萃取法均可达到类似的萃取效果。检出限为0.9 mg kg〜(-1)(k = 3,N = 8),回收率91.6-102.0%。污水污泥样品的相对标准偏差(RSD,n = 5)在1.6%和3.5%的范围内。通过对模拟土壤样品的分析验证了该方法的有效性,并将其成功应用于污水污泥实际样品中石油的测定,结果令人满意。

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