Moisture analysis

Presented by AZG team

Palupi E, Faisal A, Sulaeman A

Department of Community Nutrition – Faculty of Human Ecology – IPB

 Content
1 Introduction: why? Moisture content? Water in food?
2 Oven drying method
3 Distilation method
4 Chemical method
5 Physical method
References

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 Analysis of moisture content

1 INTRODUCTION

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 Introduction (1/2)
Why?
- Total solids: Dry matter remains after moisture removal
- Moisture is quality factor (preservation and stability): dried milk,
powdered egg, jams, glucose syrup, processed meat, etc.
- Convenience for packaging and transportation
- Computation of nutritional value
- Determination of uniform basis

Water in food?
• Free water: retains its physical properties, dispersing agent (colloid)
/solvent (salt)
• Adsorbed water: held tightly, occluded in cell walls/protoplasma
• Water of hydration: bound chemically: lactose monohydrate,
Na2SO4.10H2O

Sources: Fennema 1996, p. 323, Belitz et al. 2009, p. 8; Kusnandar 2010, p. 227; Nielsen 2010,
p. 135.
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 Introduction (2/2)
Sample handling
• Short contact to atmosphere
• Minimal friction during grinding
• Minimal headspace during storage
• Control temperature fluctuation: moist go to cold point
 RH 50%: lose 0.01% moisture in 5s
 RH 70%: lose 0.01% moisture in 10s

Sources: Fennema 1996, p. 322; Belitz et al. 2009, p. 8; Nielsen 2010, p. 135; Kusnandar 2010,
p. 223; Nielsen 2010, p. 135; Barrett and Elmore 1998, p. 2.
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 2 OVEN DRYING METHOD
• Heated under specified condition, calculated the weight loss, simultaneous is allowed
• Internationally approved
• 1 mol in 1 L  increase the boliling point 0.512oC
• Two stages is preferable
1. Liguid product: steam bath and oven drying
2. Dried product: air dried, ground, oven dried
• Decomposition of other food constituents:
1. Carbohydrate 100oC  6C + 6H2O
2. Hydrolysis  utilize the moisture, ex: sucrose
3. Volatile compounds  acetic, propionic, butyric acids, alcohols, esters, etc.
4. Oxidation of fatty acid  weight gain
5. 365oC: Critical temperature  CO2, CH4, H2O, CO

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 2 OVEN DRYING METHOD
• Temperature control:
Convection (atmospheric) (w/o fan; 10oC), forced draft (with fan ;1oC), vacuum
• Use! tongs, dessicator, prior dried the pans (3h, 100oC)
• Standard pan: 5.5cm diameter with insert cover (glass fiber disc)
• Crust/lump:
20-30 g of sand/ 3 g of sample: sand pan technique for sticky fruits
• High carbohydrate sample:
 vacuum oven (no more than 70oC, reduced pressure 25-100 mm Hg)

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 2 OVEN DRYING METHOD

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 2 OVEN DRYING METHOD
• Microwave analyzer:
1. First precise and rapid technique (10 min vs 1-16 h)
2. In process adjustment of the moisture content
Examples:
• Tomato product (AOAC 985.26)
• Meat and poultry product (AOAC 985.14)

• Infrared drying:
1. Involved penetration of heat into the sample (10-25 min)
2. High speed
3. Suitable for qualitative in-process use
4. No AOAC

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 3 DISTILLATION
• High boiling point solvent, immicible in water

Process:
• Codistilling the moisture and the solvent  collecting the mixture that
distills off  measuring the volume of the water
Classification:
• Direct and reflux distillations
• Toluene (110.6oC), Xylene (137-140oC), Benzene, Tetrachlorethylene
(121oC, no fire hazard)
• Widely used: reflux with toluene
Examples: Spices (AOAC 986.21), cheese (AOAC 969.19)
Potential error:
1. Unbreaking emulsion  need cooling
2. Clinging of water droplets to dirty apparatus
3. Water production from the decomposition of sample

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 3 DISTILLATION

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 4 CHEMICAL METHOD
KARL FISCHER TITRATON
• Application:
Low moisture food high in sugar or protein:
Dried fruits and vegetables (AOAC 967.19 E-G), candies, chocolate
(977.10), Roasted coffee, oils and fats (984.20)
• Rapid, accurate, no heat
• Involved the reduction of iodine by SO2 in the presence of water

• 1 mol water  1 mol SO2, 3 mol pyridine (C5H5N), 1 mol methanol

• 3.5 mg water = 1 ml reagent
• End point: dark-red-brown
Sources: Fennema 1996, p. 323; Belitz et al. 2009, p. 9; Kusnandar 2010, p. 207; Barrett and
Elmore 1998, p. 1.
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 Manual- (left) and automated- (right) KARL FISCHER TITRATON

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 5 PHYSICAL METHOD
1. Dielectric method:
electrical properties of the water, for
sample with moisture no more than 30-
35%, ex: cereal, grain
By measuring the change in capacitance or
resistance electricity

2. Hydrometry :
(specific gravity or density and moisture
content).
Best for one solute in a medium of water

2.1 Hydrometer (archimedes principle)

ex: beverages, sugar/salt solution
(saccharometer), milk (lactometer), .
Sources: Fennema 1996, p. 323; Belitz et al. 2009, p. 9; Kusnandar 2010, p. 207; Barrett and
Elmore 1998, p. 1.
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 5 PHYSICAL METHOD
2.2 Pycnometer
Comparing the specific grafity between sample and water
Ex: Sugar syrups (AOAC 932.14B), milk (AOAC 925.22)

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 5 PHYSICAL METHOD
3. Refractometer
How water in a sample effect the refraction of the light
Ex: syrups (AOAC 9.32.14C), fruits and fruits products (AOAC 932.12,
967.20, 983.17), soft drink, orange juice, milk

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 5 PHYSICAL METHOD
4. Infrared analysis:
Absorption at wavelengths characteristic of the molecular vibration in
water, possible at line
Ex: milk (fat, protein, lactose and total solid, AOAC 972.16)

5. Freezing point:
Physical property of sample changed
by a change in a solute concentration

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 5 PHYSICAL METHOD
1. Dielectric method: electrical properties of the water, for sample with
moisture no more than 30-35%, ex: cereal, grain
2. Hydrometry (specific gravity and moisture content). Best for one solute in
a medium of water  Hydrometer (archimedes principle) , ex:
beverages, sugar/salt solution (saccharometer), milk (lactometer), .
Pycnometer (Comparing the specific grafity between sample and water),
sugar syrups (932.14B), milk (925.22)
3. Refractometer (how water in a sample effect the refraction of the light,
ex: syrups (9.32.14C), fruits and fruits products (932.12, 967.20, 983.17),
soft drink, orange juice, milk
4. Infrared analysis (absorption at wavelengths characteristic of the
molecular vibration in water): at line, ex: milk (fat, protein, lactose and
total solid, 972.16)
5. Freezing point (physical property of sample changed by a change in a
solute concentration)
Sources: Fennema 1996, p. 323; Belitz et al. 2009, p. 9; Kusnandar 2010, p. 207; Barrett and
Elmore 1998, p. 1.
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 References
Nielsen SS. 2010. Food analysis. 4th Ed. Springer Science + Business Media, LLC: New
York, Dordrecht, Heidelberg, London.
Nielsen SS. 2010. Food analysis: Laboratory manual. 2nd Ed. Springer Science +
Business Media, LLC: New York, Dordrecht, Heidelberg, London.
Kusnandar F. 2010. Kimia pangan: Komponen makro. Dian Rakyat: Jakarta.
Andarwulan N, Kusnandar F, Herawati D. 2011. Analisis pangan. Dian Rakyat: Jakarta.
Winarno FG. 1997. Kimia pangan dan gizi. PT Gramedia Pustaka Utama: Jakarta.
Belitz H-D, Grosch W, Schieberle P. 2009. Food Chemistry. 4th revised and extended
Edition. Springer-Verlag: Berlin, Heidelberg.
Fennema OR. 1996. Food Chemistry. 3rd Ed. Marcel Dekker, Inc. : New York, Basel,
Hongkong.
AOAC International. http://www.aoac.org/
Huang T, Jander G, and de Vos M. 2011. Non-protein amino acids in plant defense
against insect herbivores: Representative cases and opportunities for further
functional analysis. Phytochemistry, Vol. 72 Issue 13, p1531-1537.
Barrett GC and Elmore DT. 1998. Amino acids and peptides. Cambridge University
Press: New York.

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 Thank you

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