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萃取分离—钙试剂[乙二醛缩双—(邻氨基酚)]萃取比色法取试样0.1克(含钙0—6微克),用1:1盐酸20毫升分解,加15%过氧化氢5毫升使铁等氧化,加热煮沸除去过氧化氢。冷却后,移入分液漏斗中,用2:1盐酸20毫升洗涤容器合并于主液中,加入甲基异丁基甲酮20毫升,激烈振荡约1分钟,静置分层后,移下层溶液于另一分液漏斗中,重复萃取至下层溶液无 Fe~(+3)的颜色为止。取出下层溶液加热煮沸除去有机物质,放冷后,加水10毫升,滴加20%氢氧化钠溶液调节 pH 至12.5。移入分液漏斗中,加入0.5%钙试剂溶液1.5毫升摇匀,立即加入正丁醇10.0毫
Extract-Calcium reagent [glyoxal bis- (o-aminophenol)] Extraction Colorimetric method Take 0.1 g of sample (0-6 μg of calcium), decompose with 20 ml of 1: 1 hydrochloric acid, add 15% Five milliliters of hydrogen and other iron oxides, boiled to remove hydrogen peroxide. After cooling, transferred to a separatory funnel, with 20: 2 hydrochloric acid 2: 1 washing container was combined in the main liquid, 20 ml of methyl isobutyl ketone was added, intense shaking for about 1 minute, after standing layered, In a separatory funnel, repeat the extraction to the lower solution without Fe ~ (+3) color so far. Remove the lower solution was heated to remove boiled organic matter, let cool, add water 10 ml, 20% sodium hydroxide solution was added dropwise to adjust the pH to 12.5. Into a separatory funnel, add 0.5% calcium reagent solution 1.5 ml shake, immediately add n-butanol 10.0 milliliters