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在炉前快速比色测定硅的钼蓝溶液中,加入硝酸银-硫酸-磷酸混合液,用过硫酸铵氧化,可以分光光度法测定锰。具体的操作步骤:称试样30mg于150ml锥形瓶中,加10ml硝酸(1+4),低温加热溶解后,加5ml 15％过硫酸铵,煮至冒大气泡,加5ml10％过氧化氢,又煮至冒大气泡,取下,加5ml碱性钼酸铵(100ml 5％钼酸铵溶液中含无水碳酸钠18g)溶液,置沸水中煮20秒,取下,加50ml 1％草酸溶液,摇匀,立即加入25ml 1.2％硫酸亚铁铵溶液,摇匀。
In the furnace fast colorimetric determination of molybdenum blue solution of silicon, adding silver nitrate - sulfuric acid - phosphoric acid mixture, with ammonium persulfate oxidation, spectrophotometric determination of manganese. Specific steps: Weigh the sample 30mg in 150ml conical flask, add 10ml of nitric acid (1 +4), low temperature heating and dissolved, add 5ml 15% ammonium persulfate, cook until large bubbles, add 5ml10% hydrogen peroxide , And boiled to take the big bubble, remove, add 5ml alkaline ammonium molybdate (100ml 5% ammonium molybdate solution containing anhydrous sodium carbonate 18g) solution, set in boiling water for 20 seconds, remove and add 50ml 1% Oxalic acid solution, shake, immediately add 25ml 1.2% ammonium ferrous sulfate solution, shake.