@article{oai:barrel.repo.nii.ac.jp:00004249, author = {片岡, 正光 and 宮下, 文秀 and 神原, 富民}, issue = {10}, journal = {分析化学}, month = {Oct}, note = {過塩素酸イオンをトリス(バトフェナントロリン)コバルト(II)錯体とのイオン対として抽出し,抽出液中のコバルトを黒鉛炉原子吸光法を用いて測定することにより過塩素酸イオンを間接定量した.抽出液はバトフェナントロリン(4,7-diphenyl-1,10-phenanthroline,以下B-phenと略記)のベンゼン溶液を用い,pH 3で抽出したところ,過塩素酸イオンの濃度が0〜5*Mの範囲で直線の検量線が得られた. A trace amount of perchlorate ion was extracted into benzene as an ion-pair with tris (bathophenanthroline) cobalt(II) cation. The cobalt(II) in the extract was determined by the aid of graphite furnace atomic absorption spectrometer, which in turn determined the concentration of perchlorate ion indirectly. The procedure for the extraction of perchlorate was as follows. To a separatory funnel 40 ml of sample solution containing less than 5 *M perchlorate, 4 ml of 5 mM sulfuric acid, 2 ml of 0.01 M cobalt ammonium sulfate and 5 ml of benzene containing 4 mM bathophenanthroline were added. The mixture was shaken for 5 min and let stand for 1 h. A 10-*l portion of the benzene extract was used for the measurement. The cobalt absorption showed the constant and maximum value in the extraction at pH 2〜4 with sulfuric acid. The calibration curve was linear for the perchlorate concentration from 0.0 to 5.0 *M. The effect of foreign ions studied at 1.6 *M perchlorate indicated that 160 *M CH_3COO-, BO_2-, F-, Cl-, and HCO_3- did not interfere. However, 160 *M of H_2PO_4-, NO_3-, NO_2-, and citrate and 1.6 *M of SCN- and anionic surfactants gave positive errors. The method was applied to the determination of perchlorate in samples of potassium chlorate.}, pages = {588--592}, title = {黒鉛炉原子吸光法による微量過塩素酸イオンの間接定量}, volume = {31}, year = {1982} }