Laboratory: Determining Moisture Content and Water Activity

INTRODUCTION

Refer to Food Analysis Laboratory manual (p19) for the Background section.

Part A:

Overall Objective

Determine the moisture content of processed cheese, cheddar cheese, parmesan cheese, dry baby
cereal, Honey Nut Cheerios, and raw almonds using forced draft, vacuum and microwave oven
methods.

Method A: Forced Draft Oven

Principle of Method

Forced draft ovens circulate air with a fan so there is a uniform distribution of heat throughout
the cavity. These ovens are known for their short startup times and quick response to
temperature changes, so once the samples are in the oven there is very little fluctuation in
temperature (<1%) throughout the cavity. However, if the drying times are too long or the
temperature is too high, one runs the risk of decomposing carbohydrates, which generate water,
or volatilizing dry matter, thus leading to false high readings in moisture. The overall principle
of the method is to heat the sample under specified conditions and the loss of weight is used to
calculate the moisture content of the sample.

Supplies

 Kraft Parmesan Cheese

 Kraft Processed Cheese
 Cheddar cheese
 Gerber Brand Rice Dry baby cereal
 General Mills Honey Nut Cheerios
 Raw Almonds
 Chickpeas (Garbanzo Beans)
 Tongs
 Spatulas for weighing
 Grater and grinder
 Petri dish
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  Desiccator
 Weighing pans-disposable aluminum open pans (pre-dried at 100°C for 24 hr)

Equipment

 Forced draft oven

 Analytical balance, 0.1 mg sensitivity

Procedure

1. Remove the pre-dried and pre-labeled pans from the desiccator with tongs. Make sure
that you have the three correct pans for your sample (e.g. baby cereal pan Rep 1 to be
placed in vacuum oven will be labeled as such: BV1). Obtain three pieces of dried
glass wool.
2. Place one sample pan and piece of glass wool on the balance and record the weight in
your notebook and class data sheet. Take out the piece of glass wool with tongs, and tare
the sample pan weight.
3. CHEESE SAMPLES MUST BE GRATED PRIOR TO WEIGHING. Place 2 g of your
assigned sample in the pan and record the weight of the SAMPLE in your notebook and
the class data spread sheet. Make sure the sample is spread in a thin layer on the bottom
of the pan and place the piece of glass wool back on top of the sample.
4. Repeat steps 2 and 3 to prepare two more replicates. You will end up with 3 replicates.
5. Place prepared samples in desiccator labeled ‘forced draft’. Once all of the samples are
collected, they will be placed into a forced draft oven at 98-100°C for 24 hr.
6. Teaching assistants will remove samples at 24 hr, and place into desiccator to cool.
YOUR GROUP WILL BE RESPONSIBLE FOR WEIGHING AND RECORDING THE
FINAL WEIGHT OF YOUR SAMPLES. THIS MUST BE DONE SOMETIME
BEFORE 4 pm ON TUESDAY or THURSDAY. ALL SAMPLES WILL BE
LOCATED IN 65 FScN.

Data and Calculations

Calculate percentage moisture (wt/wt) for each sample of your product (n =3). Report the
average % moisture of your product as well as the standard deviation and coefficient of variation.

% moisture = (wt of water in sample ) x 100

(wet basis)   (wt of wet sample)

% moisture = (wt of wet sample + wool + pan) – (wt of dried sample + wool +pan) x 100
(wet basis) (wt of wet sample)

% moisture = (wt of water in sample ) x 100

(dry basis) (wt of sample- wt of water)
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 Method B: Vacuum Oven

Principle of Method

Samples will be heated under reduced pressure to remove water. Under vacuum boiling point of
water will be reduced. The loss of weight is used to calculate the moisture content of the sample.

Supplies

 Kraft Parmesan Cheese

 Kraft Processed Cheese
 Cheddar cheese
 Gerber Brand Rice Dry baby cereal
 General Mills Honey Nut Cheerios
 Raw Almonds
 Chickpeas (Garbanzo Beans)
 Grater or grinder
 Petri dish
 Spatulas for weighing
 Desiccator
 Cold finger
 Liquid nitrogen
 Weighing pans-disposable aluminum open pans (pre-dried at 100°C for 24 hr)

Equipment

 Vacuum oven
 Vacuum pump
 Flow meter
 Analytical balance, 0.1 mg sensitivity

Procedure

1. Remove the pre-dried and pre-labeled pans from desiccator with tongs. Make sure that
you have the three correct pans for your sample.

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 2. Place one sample pan and record the weight in your lab notebook and data excel file,
and the tare the sample pan weight.
7. CHEESE SAMPLES MUST BE GRATED PRIOR TO WEIGHING. Place 2 g of your
assigned sample in the pan and record the weight of the SAMPLE. Make sure the
sample is spread in a thin layer on the bottom of the pan.
3. Repeat steps 2 and 3 to prepare two more replicates. You will end up with 3 replicates.
4. Place prepared samples in desiccator labeled ‘vacuum oven’. Once all of the samples
are collected, they will be placed into a vacuum oven at 60°C for 24 hr at 27-29
inches of Hg, with a flow rate of 120 ml/min.
5. Teaching assistants will remove samples after 5 hr, and place into desiccator to cool.
YOUR GROUP WILL BE RESPONSIBLE FOR WEIGHING AND RECORDING
THE FINAL WEIGHT OF YOUR SAMPLES. THIS MUST BE DONE
SOMETIME BEFORE 4 pm ON TUESDAY or THURSDAY. ALL SAMPLES
WILL BE LOCATED IN 65 FScN.

Data and Calculations

Calculate percentage moisture (wt/wt) for each sample of your product (n =3). Report the
average % moisture of your product as well as the standard deviation and coefficient of variation.
Use the % moisture equation in the forced draft oven data and calculations section.

% moisture = (wt of wet sample + pan) – (wt of dried sample + pan) x

100 (wet basis) (wt of wet sample)

% moisture = (wt of water in sample) x 100

(dry basis)   (wt of sample- wt of water)  

Method C: Microwave Drying Oven

Principle

The sample is heated using microwave energy, and the loss of weight is used to calculate the
moisture content of the sample.

Supplies

 Kraft Parmesan Cheese

 Kraft Processed Cheese
 Cheddar cheese
 Gerber Brand Rice Dry baby cereal
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  General Mills Honey Nut Cheerios
 Raw Almonds
 Chickpeas (Garbanzo beans)
 Petri dish
 Spatulas
 Desiccator
 Weighing pads

Equipment

 Microwave Oven, CEM Model AVC 80 (with internal balance)

Procedure

For cheese samples

1. Lift cover and place weighing pad onto balance in microwave. Tare balance.
2. CHEESE SAMPLES MUST BE GRATED PRIOR TO WEIGHING.
3. Load approx. 4 g sample onto weighing pad. Spread product into a circular single layer.
4. Analyze moisture at 80% power for 2 min.
5. Microwave will report sample weight before and after as well as % moisture.
6. Repeat steps 1-5 two more times. You will end up with 3 replicates.

For baby cereal, raw almonds, chick peas, and Honey Nut Cheerios

1. Lift cover and place weighing pad onto balance in the microwave. Tare balance.
2. Load approx. 2 g sample onto weighing pad. Spread product into a circular single layer.
3. Analyze moisture at 80% power for 3 min 30 s.
4. Microwave will report sample weight before and after as well as % moisture.
5. Repeat steps 1-5 twice. You will end up with 3 replicates.

Data and Calculations

Average the three percent moisture readings from the microwave analysis. Report the average,
standard deviation, and coefficient of variation. Review the “For your lab report” section at the
end of the addendum for complete details of what should be included in your report.

Part B

Overall Objective

Determine the moisture content and water activity of samples. In addition to the moisture
determinations by Vacuum, Forced air, and microwave oven, you will chemically determine
the food moisture content and it’s corresponding water activity.content of the ‘initial’ rice-
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 based baby cereal sample will be determined using forced draft oven, vacuum oven,
microwave oven and Karl Fischer. Moisture content and water be determined using the Karl
Fischer method, and the water activity will be measured using a Decagon instrument.

Method A: Karl Fischer Moisture Determination

Principle

The Karl Fischer titration is a chemical method for determining moisture. The water in each
sample is extracted using methanol. The extract is then titrated to determine the moisture content.

Supplies

 Kraft Parmesan Cheese

 Kraft Processed Cheese
 Cheddar cheese
 Gerber Brand Rice Dry baby cereal
 General Mills Honey Nut Cheerios
 Raw Almonds
 Chickpeas (Garbanzo beans)
 Methanol
 Dried glass vials with sealing caps
 Rotary shaker
 Small syringe (1 or 3 ml)
 Silicone rubber square

Equipment

 Karl Fischer apparatus

 Analytical balance, 0.1 mg sensitivity

Procedure

Prior to class

Samples will be prepared for students prior to analysis by weighing approx. 0.1-1.0 g into a glass
vial (in duplicate). Approx. 25 ml of methanol will be added to each and the weight of the
methanol will be recorded. Samples will be sealed and placed on a rotary shaker for a minimum
of 18 hours. A blank sample (just methanol) will also be prepared to determine the residual

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 moisture content of the methanol.

During class
1. Collect appropriate samples for your group.
2. Each sample was extracted in duplicate. Each extract will be injected in duplicate on the
Karl Fischer instrument, for a total of four data points per sample).
3. For each sample, you must record
a) The mass of the syringe before injecting the sample,
b) The mass of the syringe after injecting the sample,
c) The R value displayed by the instrument when titration is complete on class data
spreadsheet.
4. To analyze the water content of an extract on the Karl Fischer instrument:
a. Press “TITR CURRENT” then “STIR SPEED” and enter “4” from the key
pad. Wait until instrument displays “READY”.
b. Using a syringe, carefully withdraw about 1 mL of the extract without disturbing
the solids of the sample. Seal the needle with a silicone rubber square
immediately.
c. Weigh the syringe on the analytical balance. Record the syringe weight (Wbefore,
g) in the spreadsheet.
d. Press “START/STOP” button and as soon as instrument says “ADD SMPL”
quickly inject the sample, keeping the needle under the fluid level. Be careful
not to come in contact with the stir bar at the bottom of the fluid chamber.
e. Carefully remove the syringe from the instrument and seal the needle with the
same silicone rubber square immediately.
f. Re-weigh the syringe and record the syringe weight in the spreadsheet. Difference
between Wbefore and Wafter is the weight of methanol injected (g).
g. When finished the “R” and the moisture content value (µg water) will
be displayed. Record the value in the spreadsheet.
h. Rinse syringe with methanol and then repeat from step (b) for each sample and
your methanol blank.

Data and Calculations

Sample weight and methanol weight will be provided (sample preparation prior to class).
Syringe ‘before’ and ‘after’ weights and R value will be collected during class. Use this data to
fill in the spreadsheet and calculate moisture content of the samples.

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 Method B: Water activity

Principle

Water activity is defined as the vapor pressure of water above a sample divided by that of pure
water at the same temperature. Measuring the water activity involves the use of a hygrometer;
the TA will inform you of what type of hygrometer you will be using and how the instrument
will take a measurement.

Supplies

 Kraft Parmesan Cheese

 Kraft Processed Cheese
 Cheddar cheese
 Gerber Brand Rice Dry baby cereal
 General Mills Honey Nut Cheerios
 Raw Almonds
 Chick peas (Garbanzo beans)
 Petri dishes
 Decagon sample cups
 Kimwipes

Equipment

 Decagon AquaLab Vapor Sorption Analyzer (VSA)

Procedure

1. Turn on Decagon water activity instrument; allow it to warm up for at least 30 minutes.
2. Directions will be given in lab on sample preparation needed to measure water activity.
3. Make sure that the rim and outside of the sample cup are clean and dry.
4. Place cup into the sample chamber, close door, and turn vial to “read”. Machine will
beep when finished (this may take anywhere from 3-10 minutes).
5. Record the value on the class data sheet.

Data and Calculations

Water activity measurements will be recorded and averaged.

For your overall lab report (Parts A and B)

There are a number of results that you need to include in your lab report.
1) Calculate the moisture content of your product using the forced draft, vacuum, a n d
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 microwave oven on both wet and dry basis. Report the average % and coefficient of
variation of these methods. Also include a summary table of the moisture results from all
products for all methods (include the average, CV and % ERel).

2) For the sample moisture determination via the Karl Fischer, you need to calculate the
moisture content. Report the average % and CV. For water activity, calculate the average
and CV and report the results.

3) Include summary data tables.

 
4) Answer the questions about the laboratory.

Questions
1. What are the advantages and disadvantages of each method used to determine moisture
content?
2. If you need to determine the moisture content of a milk sample, which method would be
best to use? Why?
3. Compare your results to reported values and indicate which method is most accurate and
precise. Justify your answer and compare and contrast the three methods used.
4. When you need to determine food perishability, which would give you a better
indication, moisture content or water activity? Explain your answer.
5. Use your data to comment on the perishability of the different food products

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Example Summary Tables:

Wet Basis Table Forced Draft Oven Vacuum Oven Microwave Oven Karl Fisher Aw
Av C %ERe Av CV Av CV Av CV
Samples %ERel %ERel %ERel Av CV
(%) V l (%) (%) (%) (%) (%) (%)
Parmesan Cheese                            
Baby Cereal                            
Almonds C                            
Cheddar Cheese                            
Honey Nut Cheerios                            
Almonds F                            
Processed Cheese                            

 
Dry Basis Table Forced Draft Oven Vacuum Oven Microwave Oven Karl Fisher
Av CV Av CV Av CV Av CV
Samples
(%) (%) (%) (%) (%) (%) (%) (%)
Parmesan Cheese                        
Baby Cereal                        
Almonds C                        
Cheddar Cheese                        
Honey Nut Cheerios                        
Almonds F                        
Processed Cheese