2016/11/08 16:26
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方案详情:
1 实验部分
1.1 仪器和试剂
NKB3100凯氏定氮仪;XTG5201碳纤维消解仪;万分之一电子天平;
浓硫酸(98%);催化剂片(硫酸铜和硫酸钾);40%氢氧化钠;2%硼酸;0.1113mol.L-1盐酸标准滴定溶液;甲基红-溴甲酚绿混合指示剂;
1.2 方法.
1.2.1原理:样品经消化后,在碱性溶液中加热蒸馏,使氨游离蒸出,被硼酸溶液吸收,然后用盐酸标准溶液滴定并计算含量
1.2.2取样:吸取牛奶样品3.00mL于消化管中或用万分位天平用减量法称取3g于消化管中,每个消化管中再分别加入1片催化剂片,10ml浓硫酸。同时做空白。
1.2.3消解:曲线升温设置参数如下:
编号 | 温度(℃) | 时间(min) |
1 | 180 | 25 |
2 | 210 | 15 |
3 | 350 | 5 |
4 | 420 | 90 |
1.2.4蒸馏 滴定: 选择边蒸馏边滴定模式,加稀释水15ml,硼酸30ml,40%氢氧化钠40ml,蒸馏5min。
2结果讨论
样品中全氮的含量按下式计算:
式中:X1- 样品中全氮的含量(以氮计),g/100mL;
V2-滴定样品消耗0.1mol/L盐酸标准滴定溶液的体积,mL;
V1- 空白试验消耗0.1mol/L盐酸标准滴定溶液的体积,mL;
C1- 盐酸标准滴定溶液的浓度,mol/L;
0.014-1.00mL浓度是[c(HCL)=1.00mol/L]盐酸标准滴定溶液能滴定0.014g的N。
编号 | 1 | 2 | 3 | 4 | 5 |
牛奶重量 | 3.0220 | 3.2583 | 3.0530 | 3.0797 | 3.1368 |
氮白质含量% | 3.289 | 3.290 | 3.288 | 3.291 | 3.293 |
备注:标准要求做五个以上平行样,其连续5次结果的相对标准偏差在0.5%内合格。试验结果符合要求。
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