テフロンチューブを用いる銅(II) : オキシンスルホン酸錯体のインチューブ固相マイクロ抽出/電熱原子吸光法  [in Japanese] In tube solid-phase microextraction / electrothermal atomic absorption spectrometry of copper (II) using teflon tube after complexation with oxine-5-sulfonate  [in Japanese]

A Teflon tube of 1.5 m 1n 1ength and 0.5 mm ln inner diameter was used to extract Cu (II) after complexatlon with oxine-5-su1fonate 1n in-tube so1id-phase microextraetlon/electrothermal atomic absorption spectrometry. Prior to extraction, Zephiramine was 1oaded onto the inner wa1l of the Tef1on tube, the sample solution was adjusted to pH 5.6, and then p1aced ln a ca. 1 or 2-ml sample vessel. Subsequent1y, extractlon was carried out in such a way that the samp1e solution was sucked into the Teflon tube and dlscharged to the original vessel with a syringe pump included ln the auto-samp1er. The suction and discharge actions were repeated several times to attain equilibrium and to improve the amounts of copper extracted. The percent extraction after equi1ibrium was 79% for a 200-μ1 samp1e solution. The effect of the samp1e vo1ume was examlned in the range of 0.5〜2.0 m1. The suction and discharge actions were repeated 7 times with 295μl of the samp1e solution, which was the inner vo1ume of the Tef1on tube. The results showed that the amounts of copper extracted increased wlth lncreasing vo1ume of the samp1e so1ut1on up to 1.0 ml, although the percent extraction decreased with the sample volume. When copper extracted from 1.O ml of a 0.3 ng ml^<-1> sample solution was eluted by 30μl of methyl acetate (10% methanol), a reasonable repeatability with a relative standard deviation of 2.8% (n=3) was obtalned. A linaer calibration graph was also obtained in the range of 0〜0.5 ng ml^<-1> Cu(II). The detection limit (3σ) was 0.01 ng ml^<-1>. The slope of the calibration graph was 14.2-times greater than that obtained by injecting 20μl of standard solutions into the atomization furnace.