實驗二 氧化還原滴定法 預報.pdf

量不夠需再滴入若沉澱為灰色表

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量不夠需再滴入;若沉澱為灰色表 示過量,需要重新操作 ) 5. 靜置 3 分鐘,加入 20 ml Zimmermann-Rinhardt 試劑 ( 用量筒取 ) 10mL H 3 PO 4 ,稀釋至 100ml 之定量瓶中,倒入 200ml 之燒杯中 6. 先以 KMnO 4 標準液粗滴定一份褐鐵礦 ( 直到溶液呈現淺紅色 ) 並估計當量點所 需之體積
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7. 以鉑金屬當指示電極, Ag/AgCl 做為參考電極 ( 分別以去離子水沖洗 ) ,浸入溶 液中並分別以膠帶固定在燒杯壁上 8. 旋轉三用電表開關至 V ,刻度 2 。將紅色電線接頭插入伏特計的 VΩA 槽,黑 色電線接頭插於 COM 槽。紅色鱷魚夾夾在指示電極上,黑色鱷魚夾夾在參考 電極上 ( 不可夾到漆包線 ) 9. 滴定管及電極裝置好後,將燒杯至於加熱板上,放入攪拌子攪拌 ( 盡量不要打 到電極 ) 10. KMnO 4 溶液滴定第二份褐鐵礦,開始可以加入約 1~2ml 之體積變化量,讀 取伏特計之讀數並記錄之;接近當量點時,每次加入 0.1ml 的體積變化量,同 時記錄當量點顏色開始變化之體積,直到電位值呈現平緩變化為止。 四、注意事項: 1. SnCl 2 還原法分析褐鐵礦時,加熱過程應在通風櫥中進行。 2. 滴定過程當中加入 K 2 Cr 2 O 7 速度不要太快,避免超過當量點﹔假若沾到燒杯壁 上時,不要用沖洗方式將 K 2 Cr 2 O 7 沖入溶液內,此舉會改變電位值,需利用傾
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