Dhavamani, Jeyakumar, Beck, Aaron J. , Gledhill, Martha , Orif, Mohammad I., Ismail, Iqbal M.I, Achterberg, Eric P. and El-Shahawi, Mohammad S. (Submitted) An Improved Method for Measuring Phthalates in Seawater With Blank Contamination Using GC-MS. SSRN Electronic Journal . DOI 10.2139/ssrn.4219583.

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Abstract

Quantification of phthalates or phthalic acid esters (PAEs) might be problematic due to matrix overlap, auto-self absorbance and background scattering noise by the plastic lab materials although plastics have been reported in the release of PAEs. These materials (ambient air, reagents bottles, sampling devices, and various analytical instruments), are ubiquitous in the laboratory environment, thereby making it more difficult to reliably analyze of trace concentration of PAEs. Thus, in the current study, a straight forward and reliable protocol has been established for the analysis of PAEs including control of blank contamination, and the experimental conditions such as extraction time and temperature were optimized. The mass of PAEs in blank tests of selected materials ranged from 3±0.7 to 35±6 ng for liquid-liquid extraction (LLE) and from 5±1.8 to 63±15 ng for solid-phase extraction (SPE). For both extraction methods, higher blank values were measured for dibutyl phthalate (DBP) (35±6 ng, 12±3 ng), and DEHP (63±12 ng, 23±5 ng) in LLE and SPE, respectively. Average recoveries of PAEs in LLE were 90-97% and obtained with successive aliquots of 2 mL, 1 mL, and 1 mL dichloromethane (DCM). For SPE, recoveries up to 86-90% were achieved with successive aliquots of 5, 3, and 2 mL DCM at a sample flow rate of 5 mL min -1 . Under the optimized conditions, the method quantification limits (MQL) for PAEs was 10-20 ng L -1 for LLE and 10-35 ng L -1 for SPE. Moreover, the dissolved concentrations of PAEs from LDPE measured by the LLE method ranged < 1.5 to 5.83 ng cm -2, and those measured by SPE ranged from 1.0to256ngL -1 , in seawater samples of Sharm Obhur. The method has lower MQL values for LLE and SPE than average reported values of 10-100 ng L -1 and 30-100 ng L -1 , respectively.

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