Certified reference material for quantification of polycyclic aromatic hydrocarbons in sediment from the National Metrology Institute of Japan

Abstract

The National Metrology Institute of Japan has issued a certified reference material (CRM) of freshwater lake sediment for polycyclic aromatic hydrocarbon (PAHs) analyses. The certification used three extraction techniques: pressurized liquid extraction (PLE) with toluene, PLE with dichloromethane/ethyl acetate (1:1 by volume), and alkaline extraction (1 M KOH in methanol) in combination with microwave-assisted extraction. Both gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/dopant-assisted atmospheric pressure photoionization/MS (LC/DA-APPI/MS) analyses were used. Certified values are provided for 18 PAHs at 1-25 microg kg(-1) except for perylene (2.08 x 10(3) microg kg(-1)), and information values are provided for two. Since the values of PAHs in the CRM are much lower than those in other CRMs and are comparable to those found at sites with little human influence, the CRM is suitable for PAH monitoring in sediment and soil samples.

Perylene in Lake Biwa sediments originating from Cenococcum geophilum in its catchment area

“…To represent the typical Lake Biwa sediment, NMIJ CRM 7307-a (National Metrology Institute of Japan, Ibaraki, Japan) was used because it not only contains perylene at 2.1 lg g À1 (Itoh et al, 2009), but it also is possible to obtain enough of this sample for analysis. It had been prepared from sediments collected from the south basin of Lake Biwa (35°4 0 12 00 N, 135°55 0 12 00 E) in 2001 (100 kg dry wt, surface sediment to a depth of 10 m from the lake bed) (Itoh et al, 2009).…”

“…Lake Biwa is one of the best locations for field studies to elucidate the origin of perylene because its sediments commonly contain very high amounts of perylene (lg g À1 -level; Ishiwatari and Hanya, 1975;Itoh et al, 2009Itoh et al, , 2010a. These values are some of the highest concentrations of perylene found in sediment samples worldwide (Gschwend et al, 1983;Venkatesan, 1988;Jiang et al, 2000;Silliman et al, 2001;Grice et al, 2009;Suzuki et al, 2010).…”

Possible precursor of perylene in sediments of Lake Biwa elucidated by stable carbon isotope composition

“…The 100-kg sample was air-dried, pulverized, sieved to remove particles larger than 106 µm, homogenized, and subsampled into 60-g portions to form 1000 bottles. The subsamples were bottled, sterilized by γ-irradiation with 60 Co, and stored at 4°C (Itoh et al, 2009).…”

“…On the basis of the range of values for typical plant bulk samples collected in Japan (Chikaraishi and Naraoka, 2003), both values of perylene and friedelin are clearly more negative than those of aquatic plants (C 3 , -16.5‰ to -14.6‰) and the origins of perylene appear to be (C 3 ) gymnosperms, with values ranging from -28.3‰ to -26.0‰, whereas friedelin appears to originate from C 3 angiosperms, with values ranging from -37.5‰ to Perylene in Lake Biwa 165 -28.6‰. A bias in the δ 13 C value of perylene from perylene originating from other sources such as combustion can be considered negligible because the concentrations of other PAHs produced by combustion (benzo[a]pyrene: 0.0046 µg g -1 ; Itoh et al, 2009) are so clearly different from that of perylene (1.2 µg g -1 ). Since we found no friedelin in the fallen branches and leaves of typical Japanese gymnosperms such as cedar, pine, fir, and cypress in our preliminary experiments, the high amounts of both perylene and friedelin in the Lake Biwa sediments are likely to be a coincidence rather than a sign of a shared origin.…”

Experimental design approach to the optimisation of hydrocarbons extraction from the sediment: Method development and application

“…Other extraction techniques have also been developed not only in order to reduce the volume of solvents and extraction times, but also to improve precision of the analytes recoveries. Such techniques include microwave-assisted extraction (MAE), supercritical fluid extraction (SFE) and accelerated solvent extraction (ASE) (Camel, 2001;Song et al, 2002;Charriau, 2009;Itoh et al, 2009;Itoh et al, 2010). Among these techniques, ASE, also known as pressurized liquid extraction (PLE), remains an efficient tool for different solid samples extraction.…”