KARL FISCHER TITRATION METHOD
The Karl Fischer titration is a well-known analytical technique for the determination of water
content in various samples (Scholz, 1984; Aichert, 1992, Aichert, 1993, Aichert, 1998; Isengard,
1998; HYDRANAL®, 1988; Wieland, 1985). It is based on the reaction of water with iodine.
The reaction is performed in an alcoholic solution. The Karl Fischer reaction was analyzed in
detail (Scholz, 1984) and is still the object of intensive study (Cedergren, 1996; Grünke, 1998,
Grünke, 1999). Karl Fischer titration is a titration method that uses volumetric or coulometric
titration to determine the quantity of water present in a given analyte. This method for
quantitative chemical analysis was developed by the German chemist Karl Fischer in 1935. Karl
Fischer reagent consists of iodine, Sulphur dioxide, a base and a solvent, such as alcohol. In the
aqueous environment, the Bunsen reaction between iodine and Sulphur dioxide is the basis for
the reactions.
The product to be tested is combined in some fashion with chemical reagents. A chemical
reaction occurs where the water is separated chemically from the remainder of the sample. The
water is then moved to another cell where it is measured. That measurement is compared with
the initial mass or volume of the sample and moisture is calculated. (www.kett.com)
Advantages of Karl Fischer titration method
Extreme accuracy because KF titration is based upon a chemical reaction which depends
upon the presence of water.
Specificity for water determination because it does not detect the loss of any other
volatile substances unlike other methods such as loss on drying which are based upon the
heat-induced loss of moisture and the resulting reduction in weight of the sample.
Wide range of determination from 0.001 to 100%, or from 100 percent to 1 in 1 million
parts per million (ppm) with smaller percentages up to 1% being suited for coulometric
KF titration while samples with more.
Limitations of Karl Fischer titration
Manual volumetric KF titration requires reloading for each determination and hence has a
high solvent consumption.
The margin of error is relatively large when manual volumetric KF titration is applied to
materials that contain starch.
The manual titration requires considerable operator input.
Samples are destroyed or altered.
OVEN DRYING METHOD
This is also known as Loss On Drying Moisture Meter Method (LOD). The air oven-drying
method involves drying a sample in an oven and then weighing the sample before and after
drying. The difference in weight is used to calculate the amount of water present in the sample.
Tests can be manually conducted (weigh, oven dry, weigh) or automated (integrated weight and
heating unit) with systems called Moisture Determination Balances. Depending on the balance
and heating mechanism, a wide array of precision and accuracy is available. The method is
simple and does not require special equipment, but it can be time-consuming and it may not be as
accurate as other methods. Additionally, the method can be affected by factors such as the type
of oven used and the temperature at which the sample is dried.
LOD Moisture Measurement Technology
Advantages of oven drying method
It is standard conversion method.
Accommodates large number of samples.
It is a primary method hence does not require calibration.
Moisture balances are cheaper than more sophisticated instruments.
Disadvantages of oven drying method
Loss of volatile substances during drying.
Decomposition of sample e.g. sugar.
Variation of temperature due to particle size, sample weight, position in the oven.
MICROWAVE ABSORPTION
The microwave method is based on the fact that water absorbs microwave energy. This means
that the amount of energy absorbed by a sample can be used to calculate the amount of water
present. The sample is placed in a microwave oven, and the amount of energy absorbed is
measured by the detector. Based on a product calibration, the microwave energy changes into a
moisture content measurement. The method is quick and relatively simple, but it is not as
accurate as the Karl Fischer method. It also requires special equipment, such as a microwave
oven and a detector for measuring energy.
Advantages of microwave absorption method
Moisture content measurement is the representative of the entire product and is not just
measurement of surface moisture.
Nondestructive.
No extraction required and it is more accurate than low frequency resistance or
capacitance meters.
Limitations of microwave absorption method
Equipment is expensive.
Results affected by factors such as particle size, temperature, soluble salt contents,
polarization and frequency of sample.
Hard to conduct a field or an online system trial-generally must have a license and
certified specialists on site during the test.
DISTILLATION METHOD
Distillation method are based on direct measurement of the amount of water removed from a
food sample by evaporation. %moisture =100 × [M water/ M initial]. Basically, distillation
method involves heating a weighted food sample [ M initial] in the presence of an organic
solvent that is immiscible with water, the water sample evaporated and is collected a graduated
glass-tube where its volume is read. (Thiex and VanErem 2002).
Advantages of distillation method
Disadvantages of distillation method
Conclusion
Moisture content determination accuracy for food substance sample identifying a larger bulk
volume will be as precise as the representative sample quality. When choosing material samples
from a batch, the area of sample selection is crucial, for reproducible test results, test samples
must be truly representative of the entire homogeneous batch being tested. There are a lot of
moisture content determination methods in the field of food technology, so choosing a suitable
technology or technique for the specific food product is paramount. Proper amount of water in
foodstuffs is essential for controlled chemical and biological processes that may affect the
standard of the food.
