水酸化ジルコニウム共沈法による陸水中のヒ素(III)及びヒ素(V)の分別比色定量法

書誌事項

タイトル別名
  • 水酸化ジルコニウム共沈法による陸水中のひ素(III)及びひ素(V)の分別比色定量法
  • Sequential spectrophotometric determination of inorganic arsenic(III) and arsenic(V) species in groundwaters by means of coprecipitation with zirconium hydroxide
  • スイサンカ ジルコニウム キョウチンホウ ニ ヨル リクスイチュウ ノ ヒソ

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抄録

Arsenic(III) and arsenic(V) in groundwaters at ppb levels are determined by a spectrophotometric method with silver diethyldithiocarbamate (SDDC), after preconcentration by means of coprecipitation with zirconium hydroxide, and sequential generation of arsine with sodium tetrahydroborate by pH adjustment of sample solution. Three milli liters of 3.53 % zirconium oxychloride solution (30 mg as Zr) is added to 1000 ml of sample solution containing (0.510)μg of arsenic, then the solution is adjusted to pH 9 with aqueous ammonia. After standing for a while, the precipitate is collected by centrifuging, dissolved in 1 ml of 6 N hydrochloric acid solution, and transferred to a reaction vessel. Then 5 ml of 25 % tartaric acid solution is added, and the solution is adjusted to pH 6 with aqueous ammonia. The solution is diluted to about 50 ml with water, and 2 ml of Tris buffer solution is addeed to the vessel. Into the reaction vessel, 3 ml of 4 % sodium tetrahydroborate solution is injected from a funnel, and argon is bubbled at the flow-rate of (60100) ml min-1 for 20 min. Arsine generated from arsenic(III) is trapped in a SDDC solution (1). Hence 5 ml of 6 N hydrochloric acid is added to the vessel to bring the pH of the solution to 01. Three milliliters of 4 % sodium tetrahydroborate solution is injected and argon is bubbled for 15 min to generate arsine from arsenic (V). Arsine is trapped in another fresh SDDC solution (2). The concentrations of arsenic in both SDDC solutions (1) and (2) are determined by spectrophotometry at 540 nm. The recoveries of arsenic (III) and arsenic (V) are quantitative and thier coefficients of variation are about 5 % ranging (2.0 10.0)μg of arsenic, and the detection limit of arsenic is about 0.5μg. This method is rapid and convenient for the determination of trace amounts of inorganic arsenic species in groundwaters.

収録刊行物

  • 分析化学

    分析化学 33 (1), 43-48, 1984

    公益社団法人 日本分析化学会

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