Practicum 4

Moisture and ash content

A gravimetry method

Outline
Learning objectives........................................................................................................... 1
Introduction..................................................................................................................... 1
Quiz ................................................................................................................................. 3
Case study........................................................................................................................ 4

Learning objectives
1. Understand the principle of moisture and ash analysis using gravimetry method
2. Enable to calculate, analyze and interpret data of moisture and ash analysis

Introduction
Moisture analysis is one of the most important analyses performed on a nutrient analysis and
yet one of the most difficult from which to obtain accurate and precise data. The dry matter
that remains after moisture removal is commonly referred to as total solids. This analytical
value is of great economic importance to a food manufacturer because water is an inexpensive
filler. Moisture content is important parameter for food quality related to self-life, quality
itself, convenience packaging and transportation, standard of identity, nutritional evaluation,
and uniform basis. The moisture content of foods varies greatly. Water is a major constituent
of most food products. The approximate, expected moisture content of a food can affect the
choice of the method of measurement. It can also guide the analyst in determining the
practical level of accuracy required when measuring moisture content, relative to other food
constituents.

Depending on the form of the water present in a food, the method used for determining
moisture may measure more or less of the moisture present. This is the reason for official
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methods with stated procedures. However, several official methods may exist for a particular
product.

In oven drying methods, the sample is heated under specified conditions, and the loss of
weight is used to calculate the moisture content of the sample. The amount of moisture
determined is highly dependent on the type of oven used, conditions within the oven, and the

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time and temperature of drying. Various oven methods are approved by AOAC International
and SNI for determining the amount of moisture in many food products. The methods are
simple, and many ovens allow for simultaneous analysis of large numbers of samples. The
time required may be from a few minutes to over 24 h.

Ash refers to the inorganic residue remaining after either ignition or complete oxidation of
organic matter in a foodstuff. A basic knowledge of the characteristics of various ashing
procedures and types of equipment is essential to ensure reliable results. Two major types of
ashing are used: dry ashing, primarily for proximate composition and for some types of specific
mineral analyses; wet ashing (oxidation), as a preparation for the analysis of certain minerals.
Microwave systems now are available for both dry and wet ashing, to speed the processes.
Most dry samples (i.e., whole grain, cereals, dried vegetables) need no preparation, while
fresh vegetables need to be dried prior to ashing. High-fat products such as meats may need
to be dried and fat extracted before ashing. The ash content of foods can be expressed on
either a wet weight (as is) or on a dry weight basis.

Dry ashing refers to the use of a muffle furnace capable of maintaining temperatures of 500–
600◦C. Water and volatiles are vaporized, and organic substances are burned in the presence
of oxygen in air to CO 2 and oxides of N 2. Most minerals are converted to oxides, sulfates,
phosphates, chlorides, and silicates.

Materials and Tools

1. Sample: Wheat flour
2. Analytical scales (0.1mg)
3. Oven
4. Desiccator
5. Tong
6. Aluminum pan
7. Porcelain, quartz or platinum pan (30-50 ml)
8. Burner/bunsen
9. Furnace (1oC)

Work Procedures
Refer to SNI 3751: 2018 (Wheat Flour)

Moisture analysis
1. Heat an empty aluminum pan in the oven 130±3oC for 1 hour
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2. Cool the pan in a desiccator to room temperature

3. Weigh the aluminum pan and record the results (a gram)
4. Put 2 grams of the sample into the aluminum cup and weigh it (x grams) → accuracy?
5. Place the pan and its contents in the oven 130±3oC for 1 hour
6. Cool the pan and its contents in a desiccator to room temperature
7. Weigh the final weight of the cup and its contents (y grams)

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 ( x − y ) x100 %
Water content (% bb) =
( x − a)

Where:

• x = weight of empty pan and samples before drying (g)

• y = weight of plate and sample after drying (g)
• a = weight of empty cup (g)

Accuracy: The range of results for two replications is maximum 5% of the mean value of the
resulting moisture content or deviation (RSD) maximum 2%. If the range is greater than 5% or
the deviation is greater than 2% the analysis must be repeated.

Ash analysis
1. Heat the pan in furnace at 550±10°C, preheated in an electric bath / Bunsen over low
heat for 1 hour prior to put it in furnace
2. Chill in the exicator for 1 hour, then weigh (W1)
3. Weigh 3 g to 5 g sample (W2)
4. Set over low flame over an electric bath/Bunsen
5. Ashing in the furnace at 550±10°C until white or gray for 5 to 8 hours
6. Cool in an exicator for 30 minutes and weigh
7. Put back in the furnace at the same temperature for 1 hour, cool in exicator with the
same time and weigh
8. Repeat stage 7 until a fixed weight is obtained, difference in weighing the last and the
previous maximum 1 mg (W3)
9. Do a duplo
10. Calculate the ash content in the sample

Calculation:

Ash content = [(W2-W1)/W].100%

Note:

• W1 is the weight of the empty cup (g),

• W2 is the weight of the empty cup and sample (g),
• W2 is the weight of the empty cup and ash (g).
Accuracy: The range of results for two replications maximum 5% of the average value of
the ash content or deviation (RSD) maximum 3%. If the range is greater than 5% or RSD is
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greater than 3%, then the analysis must be repeated.

Quiz
The quiz can be accessed via the following link:

3
Case study
The simulation video can be accessed via the following link:

Moisture analysis
Sampling 1 Sampling 2
Replication a x y Replication a x y
1 25.2961 27.3161 27.0723 1 25.2961 27.3561 27.0523
2 25.2216 27.2321 26.9894 2 25.2217 27.2221 26.9894
3 25.5135 27.5478 27.3031 3 25.5135 27.5478 27.3031
4 25.9603 27.9785 27.7362 4 25.9604 27.9887 27.6362
5 25.5642 27.5735 27.3303 5 25.5640 27.6735 27.3303
Note:
• x = weight of empty pan and samples before drying (g)
• y = weight of plate and sample after drying (g)
• a = weight of empty cup (g)

Moisture analysis
Sampling 1 Sampling 1
Replication W1 W2 W3 Replication W1 W2 W3
1 28.0805 31.2065 28.0992 1 28.0805 31.1065 28.0972
2 24.3207 27.3300 24.3377 2 24.3207 27.3305 24.3376
3 25.2605 28.2789 25.2767 3 25.2605 28.2781 25.2765
4 26.5481 29.5590 26.5635 4 26.5481 29.5590 26.5645
5 25.4193 28.4591 25.4370 5 25.4193 28.4491 25.4360
Note:
• W1 is the weight of the empty cup (g),
• W2 is the weight of the empty cup and sample (g),
• W2 is the weight of the empty cup and ash (g).

1. Identify factors that one would need to consider when choosing a moisture analysis
method for a specific food product!
2. Why is standardized methodology needed for moisture determinations?
3. Identify the key points in the procedure of moisture and ash analysis of wheat flour
that should need to be considered to assure the data quality!
4. How to check the data quality?
5. According to the above result please check the data quality and interpret the result!
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