第1页:第五章 水分的测定
Chapter 5. Determination of moisture(第五章 水分的测定)
第2页:水分测定的意义
Section 1. General
Moisture determination is one of important and most widely used measurements in the processing and testing of foods.(水分测定是食品加工与检验中重要且应用最广的测定之一)
- Dry matter(干物质)
- Stability and quality of foods(食品的稳定性与品质)
- Chemical reactions(化学反应)
第3页:水分的存在形式
1. Water forms
- Free water(自由水)
- Absorbed water(吸附水)
- Bound water(结合水)
第4页:水分测定方法的分类
2. Methods of moisture determination
- Direct determination: remove the moisture in sample by drying, distillation and extraction.(直接法:干燥、蒸馏、萃取除水)
- Indirect determination: using sample’s density, refraction, conductivity or capacitance to measure the moisture content.(间接法:密度、折光、电导率或电容)
第5页:直接法与间接法的比较
- Direct determination: good accuracy and repetition, but spending long time.(直接法:准确度与重现性好,但耗时长)
- Indirect determination: fast and automatic, but slightly weak on accuracy.(间接法:快速、自动化,但准确度稍弱)
第6页:干燥法测定水分
Section 2. Determination of moisture
1. Drying methods
- The procedures specified in food standards generally involve thermal drying methods.(标准方法一般为热干燥法)
- The material is heated under carefully specified conditions and the loss of weight is taken as a measure of the moisture content.(规定条件下加热,以失重量衡量水分含量)
第7页:干燥法的特点
Drying methods are:
- Simple(简单)
- Relatively rapid(较为快速)
- Simultaneous analyses of large numbers of samples(可同时分析大批量样品)
第8页:干燥法的前提条件
Preconditions of drying methods
- Water is the only volatile material.(水是唯一挥发性物质)
- Water can be removed drastically.(水分可被完全除去)
- During heating, weight loss caused by chemical reactions in other components can be ignored.(加热时其他组分化学反应造成的失重可忽略)
第9页:直接干燥法
1.1 Directly drying method
- Principle: in certain temperature (95-105℃) and pressure, samples are heated in oven and the water is vaporized; the loss of weight is the moisture content.(95-105℃ 烘箱加热,水汽化,失重即水分含量)
- Applying range: there is no other volatile materials besides water, and the sample is stable when heating.(适用于除水外无其他挥发物、加热稳定的样品)
第10页:两段干燥法
For samples containing above 16% moisture
Two-stage drying method: a sample is first allowed to equilibrate with the air; a subsample is then ground for the determination of the remaining moisture.(先在空气中平衡,再研磨子样测定剩余水分)
第11页:真空干燥法
1.2 Vacuum-oven methods
- Principle: water’s boiling point is decreased under vacuum.(真空下水的沸点降低)
- Applying range: samples easily degenerative when heating above 100℃, such as fruits, vegetables, syrup, etc.(适用于 100℃ 以上易变质的样品,如果蔬、糖浆)
第12页:蒸馏法测定水分
2. Distillation methods
- Distillation with an immiscible solvent under a refluxing-type of condenser.(与不相溶溶剂在回流冷凝器中蒸馏)
- The mixture of water and immiscible solvent distills off and is collected in a measuring apparatus in which water separates and its volume can be measured.(馏出液分层后读取水的体积)
第13页:蒸馏法的适用范围
Applying range
- Samples such as cereal, dried fruit, oil and flavor.(谷物、干果、油脂、香精)
- The error caused by reduction of volatile materials and fat oxidation can be avoided.(可避免挥发性物质还原与脂肪氧化造成的误差)
- Distillation method is the only method of determining flavor’s moisture content.(是测定香精水分含量的唯一方法)
第14页:卡尔·费休滴定法
3. Karl Fischer titration
- Particularly to foods that give erratic results when heated or submitted to a vacuum.(加热或抽真空时结果不稳定的食品)
- Low-moisture foods: dried fruits and vegetables, candies, chocolate, oils and fats.(低水分食品:果蔬干制品、糖果、巧克力、油脂)
- Sugar-rich foods (sugars, honey) and foods rich both in reducing sugars and proteins.(高糖食品及富含还原糖与蛋白质的食品)
第15页:卡尔·费休反应原理
Principle:2H2O + SO2 + I2 → 2HI + H2SO4
第16页:物理方法测定水分
4. Physical methods
- Electrical methods: based on the determination of conductivity or capacitance.(电测法:电导率或电容)
- Infrared determination: based on measuring the absorption at wavelengths characteristic of the molecular vibration in water.(红外法:水分子振动特征波长的吸收)
第17页:高频电容式谷物水分仪
PM-8188 高频电容式谷物水分测量仪
第18页:近红外水分测量仪
KJT-230 近红外水分测量仪
- 在自动测定模式下每 10 秒钟显示一次平均值
- 使用近红外水分分析仪时,必须预先制作标准曲线
- 配合微机软件可显示水分值与标准曲线数据,数据范围与离散情况一目了然
第19页:红外水分测量仪
红外水分测量仪:一般的样品的话,只要十几分钟就能完成测量。
第20页:水分活度的意义
Section 3. Determination of water activity
- Water activity (Aw) can foretell the storage stability more reliably than moisture content.(水分活度比水分含量更能可靠地预示贮藏稳定性)
- AW ≈ p/p0 = ERH/100
第21页:水分活度的测定方法
Determination methods
- 1. AW determination instruments(水分活度测定仪)
- 2. Diffusing method(扩散法)
- 3. Solvent extraction(溶剂萃取法)
第22页:水分活度的测定途径