This document outlines specifications and procedures for performing a titer test to determine the fatty acid content of oils and fats. It specifies the requirements for a titer test thermometer, including its type, range, markings, standardization, and case. It also describes the necessary apparatus, which includes a stirring titer assembly. The determination procedure involves saponifying the oil or fat, separating the fatty acids, and monitoring the temperature rise while stirring the melted fatty acids in a test tube to determine the titer point.
This document outlines specifications and procedures for performing a titer test to determine the fatty acid content of oils and fats. It specifies the requirements for a titer test thermometer, including its type, range, markings, standardization, and case. It also describes the necessary apparatus, which includes a stirring titer assembly. The determination procedure involves saponifying the oil or fat, separating the fatty acids, and monitoring the temperature rise while stirring the melted fatty acids in a test tube to determine the titer point.
This document outlines specifications and procedures for performing a titer test to determine the fatty acid content of oils and fats. It specifies the requirements for a titer test thermometer, including its type, range, markings, standardization, and case. It also describes the necessary apparatus, which includes a stirring titer assembly. The determination procedure involves saponifying the oil or fat, separating the fatty acids, and monitoring the temperature rise while stirring the melted fatty acids in a test tube to determine the titer point.
This document outlines specifications and procedures for performing a titer test to determine the fatty acid content of oils and fats. It specifies the requirements for a titer test thermometer, including its type, range, markings, standardization, and case. It also describes the necessary apparatus, which includes a stirring titer assembly. The determination procedure involves saponifying the oil or fat, separating the fatty acids, and monitoring the temperature rise while stirring the melted fatty acids in a test tube to determine the titer point.
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).