CHAPTER

Introduction-General methods for

Proximate analysis is defined by H. Bennett chemists use the word "crude" before these
in the Concise Chemical and Technical three terms.
Dictionary as the "determination of a group Since aB of these determinations are
of closely related components together, e.g. empirieal, conditions of analysis must be
total protein, fat." It conventionally includes precisely stated and foBowed. Results ob-
determinations of the amount of water, tained in ash and moisture determinations are
protein, fat (ether extract), ash and fiber, with governed primarily by the temperature and
nitrogen-free extract (sometimes termed Ni- the time of subjection to heat. Protein, fat
fext) being estimated by subtracting the sum and fiber figures do not represent single con-
of these five percentages from 100. In order stituents. Any errors made in these five
to emphasize the group nature of the per- determinations are arithmetically cumulative
centage of protein, fat and fiber, many in the figure obtained for nitrogen-free extract.

Water

All foods, no matter what the method of molecules, or adsorbed on the surface of
processing, contain more or less water or colloidal partic1es. These forms of water
moisture. It comprises from 60 to 95 percent require different degrees of heat to remove-
of all natural foods. In plant or animal tissues, some water remaining at temperatures up to
it may be said to exist in two general forms: charring. This means that the phrase "percent
"free water" or "bound water". Free or moisture" is meaningless unless the method of
absorbed water, the most prevalent form, is determination is stated.
readily liberated and may be determined by
most of the methods used for the determina-
Determination of Water
tion of moisture.
Bound water is combined or adsorbed A. Oven-Drying to Constant Weight
water. This may be present as water of While there are a few methods, notably the
crystallization in hydrates or as water even Kar! Fischer titration, that determine water
more firmly bound with protein or saccharide content by a stoichiometric reaction, most

1
F. L. Hart et al., Modern Food Analysis
© Springer-Verlag New York Inc. 1971
2] Introduction-General methods for proximate and mineral analysis
methods commonly used involve the direct lid, redry 1 hour. Repeat process untilloss between
application of heat by drying the sam pie to successive dryings does not exceed 2-3 mg.
constant weight at specified temperatures and Calculate the loss of weight as moisture.
atmospheric press ures. During such pro-
cedures, hydrates may form through concen- NOTES ON OVEN MOISTURE DETERMINA-
tration rendering the water in such com- TIONS

pounds more difficult to remove by l. Products with high sugar content and meats
with high fat content should be dried in the
volatilization. Other methods involve distilla-
vacuum oven at a temperature not exceeding 70°.
tion, either directly or by azeotropic distilla-
Some sugars, e.g. levulose, decompose about 70°,
tion with an immiscible solvent. An apparatus liberating water.
house summarized the methods for moisture 2. Oven methods are not suitable for sub-
adopted by the AOAC in their 1950 (7th stances, e.g. spices, containing appreciable
Edition) Official Methods of Analysis of the amounts ofvolatile constituents other than water.
Association of Official Agricultural Chemists. 1 3. The removal ofwater from a sampIe requires
that the partial pressure ofwater in the vapor phase
Method 1-1. Moisture, Air Oven Method. be lower than that of moisture in the sampIe.
Hence some air movement is necessary. This is
DETERMINATION accomplished in an air oven by partially opening
Weigh to 1 mg accuracy 2 to 10 g, depending the vents and in vacuum ovens by a slow stream
on solids content, into a weighed metallic flat- of dried air.
bottomed dish equipped with a tight fitting cover, 4. The oven temperature varies at different sites
previously dried at 90°-100°. Loosen cover and on the oven plate, hence the precaution of placing
dry in an air oven, with vents open, for 2-3 hours the sampIe near the thermometer. The variation
at 98°-100°. Remove dish, cover and cool in a may be as much as 3° or even more in older types
desiccator; weigh so on after it reaches room of air or gravity convection ovens. The more
temperature. Return dish to oven, redry one hour modern ovens of this type are equipped with
and weigh. Repeat process until change in weight efficient thermostats and sensors and claim a
between successive dryings does not exceed 2 mg. variant within 1°.
The loss ofweight is calculated as percent moisture. 5. After drying, many substances are quite
hygroscopic; the cover should be placed tightly
Method 1-2. Moisture, Vacuum Oven Method. on the drying dish immediately upon opening the
oven, and the dish should be weighed as soon as
DETERMINA TION it reaches room temperature. This may require as
Weigh to 1 mg accuracy 2 to 10 g, depending long as an hour if a glass desiccator is used.
on solids content, into a weighed, metallic flat- Smith and Mitchell 2 have pointed out that
bottomed dish equipped with a tight-fitting cover, certain dried products are better desiccants than
previously dried at 98°-100°. Loosen cover and those used in the desiccator itself and will pick up
dry in a vacuum oven connected to a pump moisture even in a closed dish. Some desiccants
capable of maintaining a partial vacuum equiva- can be regenerated by following directions on the
lent to 100 mm or less of mercury in the oven label or in the catalog. The choice of desiccant is
chamber and equipped with a thermometer important. Concentrated sulfuric acid, anhydrous
extending into the oven chamber and near the copper sulfate, and granular calcium chloride,
sampIe dishes. Crack the stopcock of the vacuum which are commonly used, are relatively inefficient.
oven to admit a current of air (about two bubbles a Anhydrous calcium sulfate, anhydrous mag-
second) dried by passing through a sulfuric acid nesium perchlorate, anhydrous barium per-
drying tower. Dry 4 to 6 hours at 60°-70°. Stop chlorate, freshly ignited calcium oxide, anhydrous
the suction and carefully admit dried air into phosphorus pentoxide are all more efficient.
the chamber. Insert cover, remove the dish and Boiled, concentrated sulfuric acid (10th ed.
cool in a desiccator. Weigh soon after dish reaches AOAC 22.006) is one of the best, but its corrosive
room temperature. Return dish to oven, loosen properties add an element of danger.