title: Certification of butyltins and phenyltins in marine sediment certified reference material by species-specific isotope-dilution mass spectrometric analysis using synthesized 118Sn-enriched organotin compounds.
abstract: A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with gamma-ray irradiation. The material was re-mixed and packaged into 250 glass bottles (15 g each) and these were stored in a freezer at -30 degrees C. Certification was performed by use of three different types of species-specific isotope-dilution mass spectrometry (SSID-MS)-SSID-GC-ICP-MS, SSID-GC-MS, and SSID-LC-ICP-MS, with 118Sn-enriched organotin compounds synthesized from 118Sn-enriched metal used as a spike. The 118Sn-enriched mono-butyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were synthesized as a mixture whereas the 118Sn-enriched di-phenyltin (DPhT) and triphenyltin (TPhT) were synthesized individually. Four different extraction methods, mechanical shaking, ultrasonic, microwave-assisted, and pressurized liquid extraction, were adopted to avoid possible analytical bias caused by non-quantitative extraction and degradation or inter-conversion of analytes in sample preparations. Tropolone was used as chelating agent in all the extraction methods. Certified values are given for TBT 44+/-3 microg kg(-1) as Sn, DBT 51 +/- 2 microg kg(-1) as Sn, MBT 67 +/- 3 microg kg(-1) as Sn, TPhT 6.9 +/- 1.2 microg kg(-1) as Sn, and DPhT 3.4 +/- 1.2 microg kg(-1) as Sn. These levels are lower than in other sediment CRMs currently available for analysis of organotin compounds.
authors.affiliation: Environmental Standard Section, National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology, Umezono 1-1-1, Tsukuba Central 3, Tsukuba, Ibaraki, 305-8563, Japan. k-inagaki@aist.go.jp
authors.forename: Kazumi
authors.initials: K
authors.lastname: Inagaki
authors.forename: Akiko
authors.initials: A
authors.lastname: Takatsu
authors.forename: Takuro
authors.initials: T
authors.lastname: Watanabe
authors.forename: Yoshie
authors.initials: Y
authors.lastname: Aoyagi
authors.forename: Takashi
authors.initials: T
authors.lastname: Yarita
authors.forename: Kensaku
authors.initials: K
authors.lastname: Okamoto
authors.forename: Koichi
authors.initials: K
authors.lastname: Chiba
mesh_terms: D002623:Chemistry Techniques, Analytical / Q000379:methods; D019015:Geologic Sediments / Q000737:chemistry*; D007554:Isotopes / Q000032:analysis; D007564:Japan; D013058:Mass Spectrometry / Q000379:methods; D009947:Organotin Compounds / Q000032:analysis*; D011865:Radioisotope Dilution Technique; D012015:Reference Standards; D014001:Tin / Q000032:analysis*
chemical_list: D007554:Isotopes; D009947:Organotin Compounds; D014001:Tin