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CERTIFICATION.

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J DOWNES. 1963-10-26. CERTIFICATION.. https://doi.org/10.1136/bmj.2.5364.1066-c

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Certification of mono-, di-, and tributyltin compounds in marine sediment certified reference material by species-specific isotope dilution mass spectrometric analysis using synthesized 118Sn-labeled butyltins.

A new marine sediment reference material (NMIJ CRM 7301-a) for butyltins analysis was prepared and certified by the National Metrological Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). The original material of the sediment was collected at a bay near industrial activities in Japan. The sediment material was air-dried, sieved, homogenized, and packaged into 1,000 glass bottles (60 g each). Certification of NMIJ CRM 7301-a was carried out at NMIJ using two different types of species-specific isotope dilution mass spectrometry: isotope dilution-ethylation-gas chromatography/inductively coupled plasma mass spectrometry (GC/ICPMS) and isotope dilution-ethylation-gas chromatography/mass spectrometry (GC/MS). A mixture of (118)Sn-enriched monobutyltin, dibutyltin, and tributyltin was synthesized in our laboratory and was used as a spike for both techniques. Certified values are given for tributyltin (0.044+/-0.004 mg kg(-1) as Sn), dibutyltin (0.056+/-0.006 mg kg(-1) as Sn, and monobutyltin (0.058+/-0.013 mg kg(-1) as Sn), being at lower levels than currently available sediment CRMs for the analysis of organotins.

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Certified sediment reference materials for trace element analysis from the National Metrology Institute of Japan (NMIJ).

Two types of sediment reference material (NMIJ 7302-a and 7303-a) for trace elements analysis have been prepared and certified by the National Metrology Institute of Japan in the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). The original materials were collected from a bay near industrial activity in Kyushu (NMIJ CRM 7302-a; marine sediment) and from Lake Biwa (NMIJ CRM 7303-a; lake sediment). The sediment materials were air-dried, sieved, homogenized, packaged in 1000 glass bottles (60 g each), and radiation sterilized. Certification of these CRM for trace elements was conducted by NMIJ, where each element was determined by at least two independent analytical techniques. Isotope-dilution inductively coupled plasma mass spectrometry (ICP-MS) was applied for certification of all the elements except mono-nuclide elements such as As and Co. Other techniques such as ICP-MS with quadrupole mass spectrometry and sector-field mass spectrometry, inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS), were also used. Certified values have been provided for 14 elements (Sb, As, Cd, Cr, Co, Cu, Pb, Hg, Mo, Ni, Se, Ag, Sn, and Zn) in both CRM.

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