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碳酸鋰-酸不溶物的測定-重量法

整理時間:2012-11-07   熱度:1222
1   范圍                                                                

   本方法適用于工業(yè)級碳酸鋰中質量分數為0.0050%~0.020%的酸不溶物的測定。                                                                                 

2   原理                                                               

試料用鹽酸分解,加熱煮沸,冷卻。過濾,將不溶物烘干,稱重。                                                              

3   試劑

3.1鹽酸,ρ1.19g/mL。                                                               

3.2甲基橙指示劑,1g/L。                                                              

4   操作步驟                                                                                                                               

4.1試樣                                                                       

p;                                                         

    碳試樣預先在250~260℃烘干2h,置于干燥器中冷卻至室溫。                                                              

    稱取50g試樣,精確至0.01g。                                                                 

    獨立地進行兩次測定,取其平均值。

4.2測定                                                                

4.2.1將試料置于600mL燒杯中,加入200mL水、1滴1g/L甲基橙指示劑,用鹽酸中和至試液呈紅色并過量1mL,加熱煮沸5min,冷卻。

4.2.2用已恒重的4號玻璃濾堝過濾,以熱水洗滌燒杯3~4次、濾渣7~8次,于105~110℃烘干1h,稱至恒重。

5   結果計算                                                                                                                           

   按下式計算酸不溶物的含量,以質量分數表示:

                                                                                                                                  

 式中:m1—玻璃濾堝和不溶物的質量,g;                                                                

m

EM>2—玻璃濾堝的質量,g;                                                                                                                                  

m—試料的質量,g。                                                                                                                                 

6   允許差                                                           

  兩個測定值之間的差值應不大于下表所列允許差。

                                                                     %

酸不溶物質量分數

允許差

0.0050~0.0200

0.0030

7   參考文獻

[1] 國家標準GB/T 11064.11-89

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