高碳铬铁中磷的测定

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分析方法试样用过氧化钠在镍坩埚中熔融,铬、铁、磷分别被氧化为Cr(Ⅵ),Fe~(3+)和PO_4~(3-),硫酸酸化后,再以氨水沉淀Fe~(3+)和PO_4~(3-),与Cr(Ⅵ)和Ni~(2+)分离,用磷钒钼黄分光光度法测定磷。称取试样0.5克于镍坩埚中,加入5克过氧化钠搅匀,先在酒精灯上熔化,再转送马弗炉中,在700~750℃的温度下,熔3分钟后取出,并转动坩埚再继续熔6~7分钟,稍冷,放入盛有200毫升蒸馏水的500毫升烧杯中,浸出熔块,煮沸分解过氧化氢,冷却,滴加(1+1)硫酸10毫升酸化,并过量5毫升,使溶液清晰,以水稀至400毫升,加热至80~90℃(近 Analytical Methods The samples were melted with sodium peroxide in a nickel crucible. Chromium, iron and phosphorus were respectively oxidized to Cr (Ⅵ), Fe 3+ and PO 4 3-. After sulfuric acid was acidified, Fe ~ (3+) and PO_4 ~ (3-) were separated from Cr (Ⅵ) and Ni ~ (2+) and phosphorous was determined by spectrophotometry with phosphorus vanadium molybdenum yellow. Weigh the sample 0.5 grams in a nickel crucible, add 5 grams of sodium peroxide, stir, first on the alcohol lamp melting, and then transferred to the muffle furnace, at a temperature of 700 ~ 750 ℃, 3 minutes after the melt removed and Turn the crucible and then continue to melt 6 to 7 minutes, a little cold, put 200 ml of distilled water in a 500 ml beaker, leach frit, boil decomposition of hydrogen peroxide, cooling, dropping (1 +1) sulfuric acid 10 ml acidification, And an excess of 5 ml, the solution was clear, diluted with water to 400 ml, heated to 80 ~ 90 ℃ (near
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