color ta3d_64

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Page 1 of 1 INDUSTRIAL OILS AND DERIVATIVES AOCS Official Method Td 3a-64 Replaces L 15a-58 • Reapproved 1997 Color after Heating DEFINITION This method measures the color stability of fatty acids after heating under the specified conditions of the test. SCOPE Applicable to all normal fatty acids. APPARATUS 1. Oil bath—5000-mL stainless steel beaker equipped with a mechanical stirrer and containing any light-col- ored alkali-refined oil. Hydrogenated cottonseed oil is suitable for this purpose. 2. Heat source—Tirrill burners (3) are satisfactory, but electric immersion heaters with suitable thermostatic control may be used. 3. Thermometer—partial immersion, 95–255°C, AOCS Specification H 11-58. 4. Tubes—2.5 × 24 cm with ground-glass joint (see Fig. 1). Available from Kontes, Vineland, NJ USA, or any other manufacturer of special glassware (see Notes, 1). 5. Test tube holder—see Figure 2. 6. Timer—interval timer capable of measuring intervals of time up to and including 120 min. 7. Filter paper—fine porosity such as Eaton and Dikeman no. 512, Whatman no. 12, Reeve–Angel no. 871, S and S no. 596, or any equivalent filter paper. 8. Nitrogen—source of nitrogen capable of being regulat- ed to 1–2 psi pressure. PROCEDURE 1. Bring the bath to a temperature of 205 ± 2°C and maintain the temperature within the specified range. 2. If the sample to be tested is not liquid at room tempera- ture, liquefy by heating on a water bath to a tempera- ture not more than 10°C above the titer of the sample. 3. Fill a clean, dry tube to a depth of 12.7 cm with the sample, and place in the oil bath. 4. Adjust the level of the oil in the bath to 14 cm from the bottom of the tube(s). When placing several tubes in the bath, the bath temperature should not drop more than 5°C below the minimum bath temperature, and the recovery time to reach 205°C should not exceed 5 min. 5. Adjust the flow of nitrogen so that the surface of the sample is blanketed by inert gas at all times. 6. Set the timer for 60 min if the sample has an iodine value >15, or for 120 min if the sample has an iodine value of 15. 7. Remove the tube(s) from the bath and read the color immediately using AOCS Official Method Td 1a-64 and Gardner color standards. NOTES 1. Glassware cleanliness is of utmost importance. The suggested method is washing with detergent and rins- ing with reagent-grade acetone or alcohol. Dichromate solutions should not be used. / 9 / ′′ 1 / ′′ 1 / ′′ / 2 / ′′ / ′′ 1 / ′′ 2′′ 4 / ′′ T s Ts Figure 1. Details of color stability tube. 8 / ′′ 7′′ 4′′ 1′′ 6 holes 1 / ′′ dia on 4 / ′′ dia bolt circle 6 holes / ′′ dia on 4 / ′′ dia bolt circle 7 holes / ′′ dia on 2 ′′ dia bolt circle 3 holes / ′′ dia on 6 ′′ dia bolt circle 12 holes / ′′ dia on 4 / ′′ dia bolt circle Top plate 5 / ′′ dia / ′′ thick Bottom plate same as above except as noted 3 rods / ′′ dia 5 / ′′ long threaded 1 / ′′ on each end, 6– / ′′ hex. H.D. nuts hold plates Tube holder for heat stability test aluminum or stainless steel Scale: ′′ = 1 ′′ 5-L Stainless steel beaker Figure 2. Details of tube holder for heat stability test.

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Page 1: Color Ta3d_64

Page 1 of 1

INDUSTRIAL OILS AND DERIVATIVES

AOCS Official Method Td 3a-64Replaces L 15a-58 • Reapproved 1997

Color after HeatingDEFINITIONThis method measures the color stability of fatty acids after heating under the specified conditions ofthe test.SCOPEApplicable to all normal fatty acids.

APPARATUS1. Oil bath—5000-mL stainless steel beaker equipped

with a mechanical stirrer and containing any light-col-ored alkali-refined oil. Hydrogenated cottonseed oil issuitable for this purpose.

2. Heat source—Tirrill burners (3) are satisfactory, butelectric immersion heaters with suitable thermostaticcontrol may be used.

3. Thermometer—partial immersion, 95–255°C, AOCSSpecification H 11-58.

4. Tubes—2.5 × 24 cm with ground-glass joint (see Fig.1). Available from Kontes, Vineland, NJ USA, or anyother manufacturer of special glassware (see Notes, 1).

5. Test tube holder—see Figure 2.6. Timer—interval timer capable of measuring intervals

of time up to and including 120 min.7. Filter paper—fine porosity such as Eaton and Dikeman

no. 512, Whatman no. 12, Reeve–Angel no. 871, S andS no. 596, or any equivalent filter paper.

8. Nitrogen—source of nitrogen capable of being regulat-ed to 1–2 psi pressure.

PROCEDURE1. Bring the bath to a temperature of 205 ± 2°C and

maintain the temperature within the specified range.

2. If the sample to be tested is not liquid at room tempera-ture, liquefy by heating on a water bath to a tempera-ture not more than 10°C above the titer of the sample.

3. Fill a clean, dry tube to a depth of 12.7 cm with thesample, and place in the oil bath.

4. Adjust the level of the oil in the bath to 14 cm from thebottom of the tube(s). When placing several tubes in thebath, the bath temperature should not drop more than5°C below the minimum bath temperature, and therecovery time to reach 205°C should not exceed 5 min.

5. Adjust the flow of nitrogen so that the surface of thesample is blanketed by inert gas at all times.

6. Set the timer for 60 min if the sample has an iodinevalue >15, or for 120 min if the sample has an iodinevalue of ≤15.

7. Remove the tube(s) from the bath and read the colorimmediately using AOCS Official Method Td 1a-64and Gardner color standards.

NOTES1. Glassware cleanliness is of utmost importance. The

suggested method is washing with detergent and rins-ing with reagent-grade acetone or alcohol. Dichromatesolutions should not be used.

/

9 / ′′

1 / ′′ 1 / ′′

/

2 / ′′

/ ′′

1 / ′′2′′

4 / ′′

Ts

Ts

Figure 1. Details of color stability tube.

8 / ′′

7′′

4′′

1′′

6 holes 1 / ′′ diaon 4 / ′′ dia boltcircle

6 holes / ′′ diaon 4 / ′′ dia boltcircle

7 holes / ′′ diaon 2′′ dia boltcircle

3 holes / ′′ diaon 6′′ dia boltcircle

12 holes / ′′ diaon 4 / ′′ dia boltcircle

Top plate 5 / ′′ dia/ ′′ thick

Bottom platesame as aboveexcept as noted

3 rods / ′′ dia5 / ′′ long threaded1 / ′′ on each end,6– / ′′ hex. H.D. nutshold plates

Tube holder for heatstability test aluminumor stainless steelScale: / ′′ = 1′′

5-L Stainlesssteel beaker

Figure 2. Details of tube holder for heat stability test.