• What is the relationship between moisture and total solids?

Moisture + Total Solids = % (wet basis)

•Why do we need to know moisture content
–Economics (Water = Money)
–Shelf life (gained and lost water)
–Efficiency of processing (dry beans, soups etc)
–Standards of identity (flour, cheese, margarine etc)
For food analysis purposes, another important use for total solids
is for expressing data on a dry weight basis. HOW?

% Dry Weight = analyte/Total solids

• What was proximate analysis?
– Ash, Protein, Fat, Carbohydrate

• Sum of other Proximates + Moisture = ~100%

• Cucumber 96%
• Whole milk 87%
• Yogurt 89%
• Potato 80%
• Raisin 18%
• Roasted peanut < 2%
• Vegetable oil ~0%
Three (3) forms of water are present in foods.

1. Free water (a.k.a.: Free, Capillary, or Type III)

• Regular ol’ wet water, and all that comes with it. Easily
removed from foods. This water is best represented by water
activity (Aw).
2. Adsorbed water (a.k.a.: Bound or Type II)
• Tightly bound to carbohydrates and proteins. This water can
be removed, but requires careful consideration so as not to
destroy the food.
3. Water of hydration (a.k.a.: Structured or Type I)
• Held by hydrogen bonds. Food would probably be destroyed
before it could be removed.
i.e. Na2SO4 . 10H2O
 Type I Type II Type III
Hydration Absorbed Free
Relative Reactivity

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Water Activity
• Water can act as a solvent for molecular
dispersion. When water exists as a solvent, it can
be thought of as free water, not bound to any
thing and therefore available for chemical
reactions, microbial growth, and physical
changes.
• Water adsorbed (chemically bound….not absorbed like a sponge
does) can exist in mono or polymolecular layers on the internal or
external surfaces of molecules in the food.
• Proteins and starches have strong tendencies for forming such
interactions with water.
• Because fat is hydrophobic, it does not usually interact with the
water phase in food, however, there are phospholipids and
lipoproteins that associate at lipid-water interfaces and create
emulsion. What do we call these types of compounds?

Emulsifiers
• Sometimes, water can be chemically bound to
certain compounds like lactose (forming a stable
monohydrate), salts (tartrate), proteins and
polysaccharides (hydrogen bonding). This “water
of hydration” may vary from 0.5 to 30% of the
total water present. This water is particularly
difficult to remove for analytical purposes.
• Heat transfer rate (seldom a limiting factor)
• Temperature of product
• Surface area of product
• Diffusion of water through product
• Vapor pressure differences (RH at surface vs. product)
• Number of samples in oven, air exchange rate in oven,
vacuum or not, air movement in dryer, etc.
• Water can be gained or lost during sample preparation and largely
depends on RH.
• Once prepared, sample is placed in an oven.
• Analysis time can be several days at >100°C. Why?
• The basis for oven methods is that water boils at 100 °C.
Any problems with this?
• The moisture in foods is not “pure” water due to solutes.
• For each 1 g of solute added to 1L of water the boiling point will
increase 0.512 °C. Beginning to see the problem?
• As water is removed from a food, the [solute] steadily increases.
• Endpoint is when consecutive weightings are identical.
 • Pan handling. Weighting by difference.
• Pre-dry the sample prior to oven drying.
• Particle size, shape, surface area, porosity all affect the rate
of moisture removal (related to the transport of water to the
surface of the particle).
• What else besides water is removed in a heated oven?
• How do you determine the moisture of vinegar or sugar?
• Above 100°C, carbohydrates can decompose to carbon and
water (is this the water we want to analyze?)

C6H12O6 --->> 6C + 6 H2O

Question: How would lipid oxidation during moisture analysis

affect the final moisture content?
Everything you ever wanted to know about ovens, but were
afraid to ask

Convection ovens are similar to those commonly used at
home

Hot air slowly circulates in the oven chamber without the
aid of a fan

Opening the door introduces cool air which takes some time
before it comes up to temperature

Since pans or trays may block air flow, it is common to see
10 °C differences in temperature across the oven (the “Load
Effect”)

This limits the accuracy that can be obtained from this type
of oven

Forced draft ovens use a forced draft of air to
circulate the air within the oven

This results in a small difference in temperature
within the oven, often less than 1°C

This type of oven may have little or no "load
effect", which greatly improves accuracy by
stabilizing the drying rate between runs if the the
oven is full or only partially loaded

Vacuum ovens perhaps unsurprisingly uses a vacuum pump
and a heating element

Decreasing the pressure by creating a vacuum will allow
water removal at a lower temperature

This results in lower chance of other decomposition
reactions

Vacuum ovens require that the moisture removed from the
sample be vented to atmosphere, so usually there is a small
flow of air through the oven

This may result in temperature differences within the oven
• It is not only water that can evaporate
• What else can ?

• Not a big deal for many food

• Can be a big deal for others


Sand Pan Technique: Mix sample with sand to increase
surface area and prevent crusting on surface.

Microwave Drying: More rapid than oven techniques and
more expensive, but speed makes it economical for the food
industry. Problems of uneven heating.

Infrared Drying: Penetrating heat goes into the sample for
drying. Problems with uneven heating and poor accuracy.

Reflux Distillation: Moisture distilled from an immiscible
solvent. May be used for very low moisture samples.
Problems of emulsions and water droplets sticking to
glassware.
• Rapid Heating
• Temperature distribution
problems
• Good accuracy
• Programmable
temperature profile
• Expensive
• Limited sample numbers
• Rapid drying
• Weights by difference
• Wide temperature range
• Programmable
temperature profile
• Expensive, getting
cheaper
• Limited sample numbers
• One sample at a time
• Good accuracy
• Endpoint subjective
– Volumetric
– Coulometric
• Specific toward water
• Recommended for foods that have low moisture or samples that
give erratic results such as high sugar and fatty foods.
• The chemistry of the reaction (iodine reduction)
2H2O + SO2 + I2 --> H2SO4 + 2HI (Eq. 5)
Iodine reduction in the presence of sulfite.
• The reaction was modified to include methanol and pyridine to
ensure dissolution of all components in the mixture
• Dissolve sample in methanol and titrate with KFR
(iodine:sulfite:pyridine; 1:3:10)
• Each mL of KFR titrated equals 3.5 mg water.
• Endpoint is the rusty-brown color of excess iodine.
 CH3
Reflux Distillation
• Most common: Toluene distillation
• Low moisture samples
• Adsorbed water (Type II), difficult to
remove
• “Sensitive” samples
• Samples with many volatiles
ELECTRICAL
• Capacitance – measures a change in resistance to an electrical
current
• Measured against a known moisture content
• Conductivity – measures the strength of an electrical current
passed through a food.
• The lower the moisture the higher the resistance
HYDROMETERS
• Hydrometers use Archimedes principle (solids suspended in
liquids are buoyed by a force equal to the weight of water
displaced).
• Weight per unit volume is determined by using a calibrated
weight (the actual hydrometer itself)
• Measures sugar, salt, alcohol etc.