碳酸锂-酸不溶物的测定-重量法

整理时间:2012-11-07   热度:1056
1   范围                                                                

   本方法适用于工业级碳酸锂中质量分数为0.0050%~0.020%的酸不溶物的测定。                                                                                 

2   原理                                                               

试料用盐酸分解,加热煮沸,冷却。过滤,将不溶物烘干,称重。                                                              

3   试剂

3.1盐酸,ρ1.19g/mL。                                                               

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

4   操作步骤                                                                                                                               

4.1试样                                                                       

p;                                                         

    碳试样预先在250~260℃烘干2h,置于干燥器中冷却至室温。                                                              

    称取50g试样,精确至0.01g。                                                                 

    独立地进行两次测定,取其平均值。

4.2测定                                                                

4.2.1将试料置于600mL烧杯中,加入200mL水、1滴1g/L甲基橙指示剂,用盐酸中和至试液呈红色并过量1mL,加热煮沸5min,冷却。

4.2.2用已恒重的4号玻璃滤埚过滤,以热水洗涤烧杯3~4次、滤渣7~8次,于105~110℃烘干1h,称至恒重。

5   结果计算                                                                                                                           

   按下式计算酸不溶物的含量,以质量分数表示:

                                                                                                                                  

 式中:m1—玻璃滤埚和不溶物的质量,g;                                                                

m

EM>2—玻璃滤埚的质量,g;                                                                                                                                  

m—试料的质量,g。                                                                                                                                 

6   允许差                                                           

  两个测定值之间的差值应不大于下表所列允许差。

                                                                     %

酸不溶物质量分数

允许差

0.0050~0.0200

0.0030

7   参考文献

[1] 国家标准GB/T 11064.11-89

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