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41.1.

10
AOAC Official Method 942.18
Titer Test for Oils and Fats
Final Action

A. Specifications for Titer Test Thermometers

Type.Etched stem, glass.


Liquid.Mercury.
Range and subdivision.Minus 2 to +68 in 0.2.
Total length.385390 mm.
Stem.Constructed of suitable thermometer tubing of either plain
or lens front type. Diameter, plain front type: 67 mm; diameter, lens
front type: cross section of stem must be such that it will pass through
8 mm ring gage but not enter 5 mm slot gage.
Bulb.Corning normal or equally suitable thermometric glass.
Length, 1525 mm; diameter, 5.5 mm to not greater than that of stem.
Distance from bottom of bulb to 2 mark.5060 mm.
Distance to 68 mark from top of thermometer.2035 mm.
Length of unchanged capillary.Between highest graduation and
expansion chamber, 10 mm.
Expansion chamber.To permit heating to 85. Space above Hg
to be evacuated or filled with N2 or other suitable gas.
Top finish.Glass ring.
Graduation.All lines, figures, and letters to be clear-cut and
distinct. Each degree mark to be longer than remaining lines. Graduations to be numbered at 0 and at each multiple of 2.
Immersion.45 mm.
Marking."AOAC Titer Test," serial number, and manufacturers
name or trademark must be etched on stem. Words 45 mm immersion must also be etched on stem, as well as line extending around
stem 45 mm above bottom of bulb.
Scale error.Error at any point on scale must be 0.2.
Standardization.Thermometer must be standardized at ice
point and at intervals of ca 20, for condition of 45 mm immersion,
and for average stem temperature of emergent Hg column of 25.
Case.Thermometer must be supplied in suitable case on which
appears markings AOAC Titer Test, 2 to +68 in 0.2.
Note: For interpreting these specifications, following definitions
apply:
Total length is over-all length of finished instrument. Diameter is
that measured with ring gage or micrometer. Length of bulb is
distance from bottom to beginning of enamel backing. Top of
thermometer is top of finished instrument.
ASTM 36C titer test thermometer is satisfactory (Fisher Scientific
Co. or Scientific Products, Inc.).
B. Apparatus

Stirring titer assembly, as shown in Figure 942.18, consisting of


2 L beaker, 450 mL wide-mouth bottle (height 190 mm, id of neck,
38 mm), titer test tube (25 100 mm), and stirrer (23 mm od, one
end bent in form of loop, 19 mm diameter).
C. Determination

Heat 110 g glycerol-KOH solution (25 g KOH in 125 g glycerol)


to 150 in 800 mL beaker and add 50 mL oil or melted fat, previously
filtered if necessary to remove foreign substances. (Although
saponification often takes place almost immediately, continue heating and frequent stirring 15 min. Do not heat >150.)
When saponification is complete, usually indicated by perfectly
homogeneous solution, cool slightly and add 200300 mL H2O.
After complete solution of the soap, add with stirring 50 mL dilute

Figure 942.18Titer stirring assembly

H2SO4 (16 mL H2SO4 in 70 mL H2O). Heat solution, with frequent


stirring and addition of H2O if necessary, until layer of fatty acids is
completely melted and clear. Siphon off aqueous acid layer, add H2O
to fatty acids, boil 23 min, and again siphon off aqueous layer.
Repeat treatment with H2O until wash H2O is neutral to methyl
orange. Remove fatty acids so as not to include H2O, and filter while
melted through rapid paper. Heat to 130 on hot plate to remove
traces of H2O and pour fatty acids into titer tube to height of 57 mm
from bottom. If H2O is present in fatty acids, decant, refilter, and
reheat.
Fill H2O bath and adjust to 20 for all samples with titers 35,
and to 1520 below titer for samples with titers <35. (H2O level
should be 1 cm above sample level.) Place test tube containing fatty
acids in apparatus, Figure 942.18. Insert thermometer to immersion
mark and equidistant from sides of tube. Stir vertically with stirring
rod at rate of 100 complete up-and-down motions/min, starting
agitation while temperature is 10 above titer point. (Stirrer should
move through vertical distance of ca 3.8 cm. If preferred, stirring
may be performed mechanically.) Continue stirring until temperature remains constant 30 s or begins to rise in <30 s interval.
Immediately discontinue stirring and observe rise in temperature.
Report as titer highest point reached by thermometer. Duplicate
determinations should normally agree within 0.2.
Reference: JAOAC 25, 726(1942).

Copyright 1998 AOAC INTERNATIONAL