Sediment certified reference materials for the determination of polychlorinated biphenyls and organochlorine pesticides from the National Metrology Institute of Japan (NMIJ)

Abstract

Two marine sediment certified reference materials, NMIJ CRM 7304-a and 7305-a, have been issued by the National Metrology Institute of Japan in the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) for the determination of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs). The raw materials of the CRMs were collected from a bay near industrial activity in Japan. Characterization of these CRMs was conducted by NMIJ, where the sediments were analyzed using multiple analytical methods such as pressurized liquid extraction (PLE), microwave-assisted extraction (MAE), saponification, Soxhlet extraction, supercritical fluid extraction (SFE), and ultrasonic extraction; the target compounds were determined by one of the primary methods of measurements, isotope dilution-mass spectrometry (ID-MS). Certified values have been provided for 14 PCB congeners (PCB numbers 3, 15, 28, 31, 70, 101, 105, 138, 153, 170, 180, 194, 206, 209) and 4 OCPs (gamma-HCH, 4,4'-DDT, 4,4'-DDE, 4,4'-DDD) in both CRMs. NMIJ CRM 7304-a has concentrations of the contaminants that are a factor of 2-15 greater than in CRM 7305-a. Both CRMs have information values for PCB homolog concentrations determined by collaborative analysis using a Japanese official method for determination of PCBs. The total PCB concentrations in the CRMs are approximately 920 and 86 microg kg(-1) dry mass respectively.

Supercritical fluid extraction of polyhalogenated pollutants from aquaculture and marine environmental samples: A review

“…Another comparison between SFE and other techniques for the extraction of organohalogenated pollutants from marine sediment samples was described by Numata et al [66]. In this paper, different extraction techniques (PFE, MAE, saponification, Soxhlet extraction, SFE and ultrasonic extraction) were employed for the determination of PCBs and OCPs in two marine sediments CRMs (NMIJ CRM 7304-a and 7305-a).…”

“…The method developed showed a good performance in the determination of organochlorine compounds from freeze-dried fillets, but it did not efficiently extract these compounds from fresh fish. These results would suggest that the presence of water in the sample decreases CO 2 [66] and therefore inhibits contact between the supercritical fluid and the analytes. The SFE methodology was also compared with Soxhlet extraction, producing comparable results.…”

“…Pressurised fluid extraction (PFE) or accelerated solvent extraction (ASE) offer the sequential extraction of multiple samples in an automated system, but the drawbacks are a substantial initial capital investment, specific sample treatment for soils with high sulphur content, more solvent than SFE and external clean-up steps [61,66].…”

“…During the SFE step, many interfering components, such as large amounts of elemental sulphur, are coextracted from sediment samples together with the target analytes; so a clean-up procedure is generally required before the final chromatographic determination [25]. The simplest treatment that can be used on the sample to eliminate sulphur consists of a mixture of copper powder directly activated in the extraction cell [20,66,76]. Among the different extraction methods used for the certification of 14 PCB congeners and 4 OCPs in the new reference materials certified (NMIJ CRM 7304-a and NMIJ CRM 7305-a) [66], SFE stands out from the other procedures owing to its simplicity and high specificity.…”

“…The simplest treatment that can be used on the sample to eliminate sulphur consists of a mixture of copper powder directly activated in the extraction cell [20,66,76]. Among the different extraction methods used for the certification of 14 PCB congeners and 4 OCPs in the new reference materials certified (NMIJ CRM 7304-a and NMIJ CRM 7305-a) [66], SFE stands out from the other procedures owing to its simplicity and high specificity. Another method involving SFE with a solid phase trap containing activated alumina was investigated for the rapid analysis of polychlorinated dibenzo-p-dioxins (PCDDs), PCDFs, and dioxin like PCBs (DL-PCBs) in soils and sediments [23].…”