バッチ式固相抽出法による海水中有機スズ化合物の分離濃縮

• 郡 宗幸

  科学技術庁金属材料技術研究所

• 佐藤 幸一

  科学技術庁金属材料技術研究所

• 井上 嘉則

  横河アナリティカルシステムズ(株)

• 井出 邦和

  科学技術庁金属材料技術研究所

• 大河内 春乃

  科学技術庁金属材料技術研究所

書誌事項

タイトル別名

• Batch operation of solid phase extraction for separation and concentration of organotin compounds in seawater.
• バッチシキ コソウ チュウシュツホウ ニヨル カイスイチュウ ユウキ スズ カ

抄録

For the speciation of ultra trace organotin compounds, a batch technique for solid phase extraction (SPE) has been developed using a polymer of styrene derivative/metacrylic ester (Excel-pack SPE-GLF, Yokogawa Analytical Systems Inc., Japan) as a solid phase sorbent. The recovery of organotin compounds was measured by miceller liquid chromatography/inductively coupled plasma mass spectrometry (MLC/ICP-MS). The mobile phase was 40 mM tris(hydroxymethyl)amino methane dodecyle sulfate, 75 mM ammonium nitrate, 3%v/v acetic acid, and 20%v/v ethanol solution. The procedure was as follows. Add 0.5 g SPE sorbent suspended in 10 ml methanol into seawater samples (031) which was previously acidified to pH 2 with hydrochloric acid. After shaking for 5 min in a separating funnel, pour the solution with sorbent into a 8 ml reservoir at a flow rate of ca. 50 ml min^-1. Wash the sorbent with 20 ml of 10%v/v methanol. Elute organotin compounds by gravity flow of 12 ml methanol. Evaporate the methanol effluent to 1.0 g at 3035°C under argon gas flow. Add 1.0 g of ultra pure water. Inject 100μl of the solution into the MLC/ICP-MS. The recoveries of TPT and TBT were almost 100%, while those of DPT and DBT were lower. The batch technique was very rapid taking only ca. 20 min for the SPE of 1000 ml of seawater. The limit of detection (LOD, 3σ) of SPE/MLC/ICP-MS was TBT: 5 ng l^-1 and TPT: 7 ng l^-1, respectively, when using 1000 ml of seawater. It was also possible to perform the analysis for an effluent that was concentrated to 0.25 ml and the same volume of ultra pure water was added. Then 100 μl of the solution was injected to MLC/ICP-MS. Consequently, the LOD for this case will be much lower. The enrichment factor was 10³10⁴. The cartridge technique of SPE was also comparatively studied.

収録刊行物

• 分析化学

  分析化学 44 (7), 537-542, 1995

  公益社団法人 日本分析化学会

キーワード

• solid phase extraction of organotin compounds in seawater
• batch operation for solid phase extraction
• polymer of styrene derivative metacrylic ester as solid phase sorbent
• miceller liquid chromatography/inductively coupled plasma mass spectrometry

詳細情報

• CRID: 1390001204052499072
• NII論文ID: 110002906965
• NII書誌ID: AN00222633
• DOI: 10.2116/bunsekikagaku.44.537
• COI: 1:CAS:528:DyaK2MXmvFShu70%3D
• NDL書誌ID: 3627853
• ISSN: 05251931
• Web Site: https://ndlsearch.ndl.go.jp/books/R000000004-I3627853
• Web Site: http://www.jstage.jst.go.jp/article/bunsekikagaku1952/44/7/44_7_537/_pdf
• Web Site: http://dl.ndl.go.jp/info:ndljp/pid/10893631
• 本文言語コード: ja
• データソース種別:
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  • NDL
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  • CiNii Articles
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