このエントリーをはてなブックマークに追加
ID 19899
Eprint ID
19899
FullText URL
Title Alternative
Simultaneous determination of nitrate and nitrite ion by micro-flow injection analysis
Author
Ma, Lan
Oshima, Mitsuko
Motomizu, Shoji
Hattori, Takayasu
Abstract
To minimize the sample size, reagent consumption and waste, a micro-flow injection analysis (μFIA) was investigated and applied to the simultaneous determination of nitrate and nitrite ion in water samples. A double-plunger micropump was used to propel a carrier and a chromogenic solution; each flow rate was 50 μl min(-1), and the delivery volume was 2.5 μl per stroke. Nitrate was reduced to nitrite on line by passing through a mini column (0.53 mm i.d.×5 cm) packed with powdered Cd/Cu (6080 mesh). The reduction efficiency was 99% using this reduction column. Detection was carried out at 538 nm with a light-emitting diode used as an azo dye. The carrier solution contained EDTA and NaCl (pH 8.18.4) and the reagent solution contained sulfanilamide, N-(1-naphthyl)ethylenediamine and HCl. For a simultaneous determination, the sample injected into the carrier stream was split into two streams: one passed through the mini Cd/Cu column ; the other passed through a bypass column packed with glass beads. The sample zone passing through the bypass column gave a first peak derived from nitrite; the other sample zone passing through the reduction column gave the second peak derived from nitrate and nitrite. The detection limits of nitrate and nitrite were about 1×10(-7) M using the proposed simultaneous determination system.
Abstract Alternative
試薬,試料量の低減化とオンサイト分析を目的として,マイクロフロー方式FIA(μFIA)による硝酸イオン,亜硝酸イオンの定量について検討した.流路は二流路とし,ダブルプランジャー型マイクロポンプを用い,吐出量は2.5μl stroke-1,流量は50μl min-1とした.吸光検出反応には,スルファニルアミドと2-ナフチルエチレンジアミンを用いるジアゾ化-カップリング反応を用い,538nmで測定した.試料注入量20μlで,内径0.25mm,長さ75 cmの反応コイルを用いれば,通常の河川水程度の硝酸,亜硝酸イオンの定量が可能である.μFIA用のCd/Cu還元ミニカラムは,カドミウムパウダー(60~80メッシュ)を銅コーティングし,内径0.53mmのシリカチューブ(長さ5cm)に詰めて作製した.本ミニカラムによる硝酸イオンの亜硝酸イオンへの還元効率は99%以上であった.スプリット方式により,硝酸亜硝酸イオンの同時定量用流路を構築した.実際試料のオンサイト分析装置には,発光ダイオード(LED)を川いて,消費電力の低減化を計った.硝酸,亜硝酸イオンを単独に定量する場合の検出限界はそれぞれ約2×10(-8)Mであり,同時定量の場合には約10(-7)Mであった.河川水中の硝酸,亜硝酸イオンの同時定量にも応用できることが分かった.
Keywords
micro-flow injection analysis
river water, nitrate and nitrite
simultaneous determination
mini Cd/Cu reduction column
Published Date
1998-06-05
Publication Title
分析化学
Publication Title Alternative
Bunseki Kagaku
Volume
volume47
Issue
issue6
Publisher
日本分析化学会
Publisher Alternative
The Japan Society for Analytical Chemistry
Start Page
375
End Page
380
ISSN
0525-1931
NCID
AN00222633
Content Type
Journal Article
Official Url
http://www.journalarchive.jst.go.jp/japanese/jnlabstract_ja.php?cdjournal=bunsekikagaku1952&cdvol=47&noissue=6&startpage=375http://www.journalarchive.jst.go.jp/japanese/jnlabstract_ja.php?cdjournal=bunsekikagaku1952&cdvol=47&noissue=6&startpage=375
language
日本語
Copyright Holders
The Japan Society for Analytical Chemistry
File Version
publisher
Refereed
True