Inagaki Kazumi, Takatsu Akiko, Watanabe Takuro, Aoyagi Yoshie, Yarita Takashi, Okamoto Kensaku, Chiba Koichi
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.
Anal Bioanal Chem. 2007 Apr;387(7):2325-34. doi: 10.1007/s00216-006-0677-x. Epub 2006 Jul 28.
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.
一种用于丁基锡和苯基锡分析的新型海洋沉积物标准参考物质NMIJ CRM 7306-a已由日本国立计量院在国立先进工业科学技术研究所（NMIJ/AIST）制备并认证。候选沉积物材料取自日本一个靠近工业活动的海湾。经过风干、筛分和混合后，该材料用伽马射线辐照进行灭菌。材料重新混合后装入250个玻璃瓶（每个15克），并储存在-30℃的冷冻室中。认证采用三种不同类型的物种特异性同位素稀释质谱法（SSID-MS）——SSID-GC-ICP-MS、SSID-GC-MS和SSID-LC-ICP-MS，使用由富集118Sn的金属合成的富集118Sn的有机锡化合物作为内标。富集118Sn的单丁基锡（MBT）、二丁基锡（DBT）和三丁基锡（TBT）作为混合物合成，而富集118Sn的二苯基锡（DPhT）和三苯基锡（TPhT）则单独合成。采用了四种不同的萃取方法，即机械振荡、超声、微波辅助和加压液体萃取，以避免样品制备过程中因非定量萃取以及分析物的降解或相互转化而可能导致的分析偏差。在所有萃取方法中均使用了托酚酮作为螯合剂。给出的认证值为：TBT以Sn计为44±3微克/千克，DBT以Sn计为51±2微克/千克，MBT以Sn计为67±3微克/千克，TPhT以Sn计为6.9±1.2微克/千克，DPhT以Sn计为3.4±1.2微克/千克。这些含量低于目前可用于分析有机锡化合物的其他沉积物标准参考物质。
