@article{oai:barrel.repo.nii.ac.jp:00004256,
 author = {田村, 徹 and 片岡, 正光},
 issue = {11},
 journal = {分析化学},
 month = {Nov},
 note = {トリス(バソフェナントロリン)鉄(II)と過塩素酸イオンのイオン対を感応物質とするポリ塩化ビニル固化膜型過塩素酸イオン選択性電極を試作し,その電極特性を検討するとともに,同電極を指示電極に用い第四級アンモニウム塩のゼフィラミンを滴定剤として沈殿電位差滴定を行った. 作製した電極は10^<-1>〜10^<-6>Mの過塩素酸イオンにほぼNernst応答し,目的イオン濃度10^<-4>M溶液の電位はpH1〜13の範囲で一定であった.滴定においては,24.87〜74.60mgの過塩素酸イオンを0.6%以下の相対誤差と0.2%以下の相対標準偏差で簡便かつ迅速に定量が可能であった.実試料で過塩素酸イオンと共存することの多い硝酸イオンは正の誤差を与えるとともに,終点付近での電位飛躍を抑え,終点の判読を困難にしたが,酢酸酸性で粉末亜鉛を加え加熱し,硝酸イオンを選択的に還元することにより,その妨害を除去することが可能であった.本法を用いて実試料を分析した結果は,JIS法による分析結果と良い一致を示した.
The construction of a perchlorate ion-selective electrode and its application to potentiometric titration of perchlorate ion in the explosives with Zephiramine was described. The PVC matrix membrane containing 7.7 (w/w)% of tris-(bathophenanthroline)iron (II) perchlorate ion-associate was used as an ion-sensing membrane. The disk membrane was affixed to a PVC tube (I.D. 7 mm) and silver-silver chloride electrode was used as the internal reference electrode. The composition of the cell including the present ion-selective electrode is as follows. Ag-AgCl electrode/reference solution, 50 mM NaClO4 in 50 mM NaCl/PVC ion-exchange membrane//sample solution/SCE The present ion-selective electrode exhibited a Nernstian response to perchlorate ion in the concentration range from 10^<-6> to 10^<-1> M. The potential of the electrode was constant over the pH range from 1 to 13. Selectivity coefficients were evaluated and the electrode exhibited a good selectivity with respect to most common anions, while it showed some interferences with respect to periodate, iodide, and thiocyanate ion. The present ion-selective electrode was successfully adopted to the potentiometric precipitation titration of perchlorate ion with Zephiramine. It was revealed that the presence of equal or excess amounts of nitrate ion in the sample solution lowered the potential break at the end-point. However, the interference can be eliminated by the reduction of nitrate ion by heating with acetic acid and zinc powder.},
 pages = {591--596},
 title = {ポリ塩化ビニルをマトリックスとした液膜型過塩素酸イオン選択性電極を用いる過塩素酸イオンのゼフィラミンによる沈殿電位差滴定},
 volume = {33},
 year = {1984}
}