实验:铵态氮肥含氮量测定(请给出详细过程)

2025-04-02 11:36:46
推荐回答(2个)
回答1:

实验目的:

1.了解弱酸强化的基本原理。

2.掌握甲醛法测定氨态氮的原理及操作方法。

3.熟练掌握酸碱指示剂的选择原理。

实验原理:

由于铵盐中NH4+的酸性太弱Ka=5.6X10—11故无法用NaOH标准溶液直接滴定,可将硫酸铵与甲醛作用,定量生成质子化的六次甲基四胺和H+,反应如下:

4NH4+ + 6HCHO → (CH2)6N4H+ + 3H+ + 6H2O

所生成的(CH2)6N4H+ ( Ka = 7.1 × 10-6)和H+可用NaOH标准溶液进行滴定。滴定反应为:

(CH2)6N4H+ + 3H+ + 4OH- → (CH2)6N4 + 4H2O

由上述反应可知,4mol(NH4)2SO4与甲醛作用,生成3mol H+(强酸)和1mol (CH2)6N4H+ 离子,即lmolNH4+相当于1mol NaOH。

实验内容:

1.甲醛溶液的处理

甲醛中常含有微量酸,应事先除去。其方法如下:取原瓶甲醛上层清液40mL于烧杯中,用水稀释一倍,加2~3滴酚酞指示剂,用NaOH滴定至微红。

2.(NH4)2SO4试样中含氮量的测定

准确称取0.2~0.3g试样三份,分别置于250mL锥形瓶中,加20~30mL水溶解,加2滴甲基红指示剂,用 0.1 mo1·L—1NaOH中和后(滴至溶液由红色变为黄色),加入10mL处理后的甲醛溶液,再加2滴酚酞指示剂,充分摇匀,放置一分钟后,用0.1 mo1·L—1NaOH标准溶液滴定至溶液呈淡红色,30s不褪色,即为终点,根据用去的NaOH的体积计算试样含氮量。

注意事项

试样中含有游离酸,加甲醛之前应事先以甲基红为指示剂,用NaOH溶液中和,以免影响测定。

回答2:

称取1克试样,称准至0.0002克,置于250毫升锥形瓶中,用100~120毫升水溶解,加1滴甲基红指示剂,用0.1N氢氧化钠标准溶液或0.1N硫酸标准溶液调节至溶液呈橙色。加入15%毫升25%甲醛溶液至试液中,再加入3滴酚酞指示剂溶液,混匀,放置5分钟,用0.5mol/L氢氧化钠标准溶液滴定至与pH8.5的颜色参比溶液所呈现的颜色相同(滴定后体积约150毫升),经1分钟不消失为终点(或滴定至pH8.5)。同时作空白试验。
氨态氮含量百分数按下式计算:
x=c(V1-V2)*0.01401*100/m
式中:c-氢氧化钠标准溶液的当量浓度;
V1-滴定试样用去氢氧化钠标准溶液的体积,毫升;
V2-空白试验用去氢氧化钠标准溶液的体积,毫升;
m-试样的质量,克;
0.01401-每毫克相当量氮的质量,克。

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