浮選分離-還元気化原子吸光法による海水中のヒ素の定量

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A rapid and precise method is described for the separation and determination of arsenic in natural sea water. The procedure is as follows: Add 2 ml of iron(III) solution (5 mg ml^<-1>) to 250 ml of sea water in a 300-ml beaker. Adjust the pH to 8〜9 with aqueous ammonia solution, and stir the solution for 15min. After adding 1 ml of sodium oleateethanol solution (1 mg ml^<-1>), transfer the contents of the beaker to a flotation cell (24 × 4.8cm i.d.) fitted with a sintered-glass filter (No. 4). Pass air at 50 ml min^<-2> from the lower end of the cell about 1 min. Suck off the mother liquor through the sinteredglass disk. Add 5 M hydrochloric acid to dissolve the precipitate, collect the filtrate by suction in a 10-ml calibrated flask and dilute to 9 ml. Add 0.5 ml of 20% (w/v) potassium iodide solution into the flask prior to analysis and dilute to the mark with water. Transfer 1 ml of 5 % (w/v) sodium borohydride solution into a hydride generating cell. Inject 1 ml of sample solution containing less than 0.10μg of arsenic into the cell. Sweep the arsine thus generated into the long absorption cell (60 × 1.2 cm i.d.) with nitrogen so that it is atomized in the nitrogen-hydrogen flame and measure the absorption signal of arsenic by atomic absorption spectrophotometry. The potassium iodide pretreatment after the separation eliminated suppressive effects by diverse ions such as Cu^<2+,> Se^<4+> and Ni^<2+> in the determination of arsenic. In the analytical process, mean recoveries were (99〜101)% for arsenic (III, V) added to natural sea waters. The relative standard deviations of 7 replicate analyses of sea water samples were less than 3%.
社団法人日本分析化学会の論文
1979-09-05

浮選分離-還元気化原子吸光法による海水中のヒ素の定量

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