LUBRIZOL STANDARD TEST PROCEDURE

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Lubrizol Advanced Materials, Inc. / 9911 Brecksville Road, Cleveland, Ohio 44141-3247 / TEL: 800.379.5389 or 216.447.5000

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The information contained herein is believed to be reliable, but no representations, guarantees or warranties of any kind are made as to its accuracy, suitability for particular applications or the results to be obtained therefrom. The information is based on laboratory work with small-scale equipment and does not necessarily indicate end product performance. Because of the variations in methods, conditions and

equipment used commercially in processing these materials, no warranties or guarantees are made as to the suitability of the products for the application disclosed. Full-scale testing and end product performance are the responsibility of the user. Lubrizol Advanced Materials, Inc. shall not be liable for and the customer assumes all risk and liability of any use or handling of any material beyond Lubrizol Advanced

Materials, Inc.’s direct control. THE SELLER MAKES NO WARRANTIES, EXPRESS OR IMPLIED, INCLUDING, BUT NOT LIMITED TO, THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE. Nothing contained herein is to be considered as permission, recommendation, nor as an inducement to practice any patented invention without permission of the patent owner.

TEST PROCEDURE AATM 111C-02 Edition: October 17, 2006

Previous Edition: May 29, 2000

HYDROXYL VALUE (HINDERED HYDROXYLS)

DEFINITION This method determines the number of hydroxyl groups present which can be acetylated under the conditions of this test. It is useful for determining hindered (secondary or tertiary) hydroxyl groups which are not acetylated in the pyridine - acetic anhydride system described in AATM 111A.

Hydroxyl value is defined as the number of milligrams of potassium hydroxide necessary to neutralize the acetic acid which combines on the acetylation of one gram of sample.

DESCRIPTION OF METHOD

A specified weight of sample is acetylated by heating at 70-72° C for one hour with a measured amount of acetic anhydride in an ethyl acetate solution which contains p-toluenesulfonic acid as catalyst. The hydroxyl groups react with the acetic anhydride to form the acetate and free acetic acid. At the end of the reaction period, all the unconsumed acetic anhydride is hydrolyzed to free acetic acid by the addition of water (and pyridine), and heated for ten minutes to insure complete hydrolysis. The sample and a corresponding reagent blank which has been run at the same time are titrated with 0.5N methanolic potassium hydroxide. A mixed indicator consisting of cresol red and thymol blue is used for the titration. The difference between the blank and the sample titrations represents the amount of acetic acid consumed by the sample. The hydroxyl value is calculated (by definition) as the equivalent milligrams of potassium hydroxide per gram of sample. The amount of potassium hydroxide consumed by the free acids present in the sample must be included in the calculations. Excess acetic anhydride is required to drive the reaction to completion. Therefore, special attention must be paid to the ratio of sample size to reagent as set forth in the table shown in the procedure.

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APPARATUS 1. 250 ml ground neck erlenmeyer flasks, TS 24/40, with air condenser. 2. Controlled oil bath regulated to maintain the temperature at 70-72° C. 3. Cooling bath. ( Shallow water-filled pan). 4. Class A volumetric pipette calibrated to deliver 5 (±0.03) ml or appropriate dispenser. 5. Analytical balance capable of weighing to the nearest 0.1 mg. 6. Burette (50 ml) Class A with a tolerance of ±0.05 ml. 7. Assorted Mohr pipettes, graduated cylinders, droppers. 8. Magnetic stirrer, stirring bars. REAGENTS AND SOLUTIONS 1. Acetic Anhydride Reagent - 60ml acetic anhydride, 7.2g p-toluenesulfonic acid and 180ml

ethyl acetate. 2. Pyridine-water solution - Approximately 3ml pyridine for each 1ml water. 3. Cresol Red-Thymol Blue Indicator Solution - 1 part Cresol Red (0.1% in H2O)+3 parts Thymol

Blue (0.1% in ethanol). 4. Methanolic potassium hydroxide 0.5N- Commercially available or AATM 1002. PROCEDURE It is recommended that all blanks and sample be run in duplicate. 1. Accurately weigh the specified amount of sample into a 100 ml acetylation flask according to

the following table and record weight to the nearest 0.1 mg. Hydroxyl value Sample Size 0-20 5.0g (±0.1) 20-100 2.0g (±0.1) 100-150 1.5g (±0.1) 150-200 1.0g (±0.05) 200-250 0.75g (±0.05) 2. Into each flask, accurately add 5 ml of acetic anhydride reagent and attach an air condenser. At

the same time set up reagent blanks, containing no sample but the corresponding volume of reagent.

3. Place the flasks in the 70-72° C oil bath, immersing to the liquid level. Swirl vigorously until all the solid material is melted and is thoroughly mixed into the solution.

4. Continue heating at 70-72° C for one hour, swirling the flasks frequently to insure uniform reaction.

5. Remove the flasks from the oil bath and cool for at least ten minutes in a room temperature shallow water bath.

6. To each flask through the air condenser, using a Mohr pipette, add 2 ml of deionized water. 7. Using a Mohr pipette, add 10 ml of pyridine-water solution (reagent) to each flask through the

air condenser.

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8. Swirl vigorously to mix thoroughly. Return the flasks to the oil bath for 10 minutes to complete

the hydrolysis of the excess acetic anhydride reagent. Swirl at frequent intervals. 9. Remove the flasks from the oil bath and place them in the cooling bath for at least ten

minutes. 10. Remove the condenser. Using a dropper, add 1 ml of the indicator solution. Add a magnetic stirring bar. 11. Fill burette and titrate the blanks and the samples using 0.5 N methanolic potassium hydroxide.

NOTE: The end point color of the blank is a bold blue color with no trace of red when viewed against the light. The end point color of the sample will vary to some extent depending upon the color of the test sample. The final color is usually a deep gray blue with the disappearance of the last traces of red color marking the end point. The sample should be heated under hot water to release any remaining occluded traces of acid just before the end of the titration.

An alternate method may be used by adding (by pipette) 10 ml pyridine to each flask just before titration. This is found to be preferable by some analysts who feel that it improves the sharpness of the end point. Either method of titration may be used only if all samples and blanks receive identical treatment.

12. Read the burette to two decimal places and record the mls used by all samples and

blanks. 13. Determine the acid value of the sample (AATM 109). CALCULATIONS Hydroxyl value = (ml KOH blank - ml KOH sample) X N KOH X 56.1 + acid value g sample

PRECISION

Product Average Std Dev Coeff of Var df Cm

Cremerol 35.01 1.186 3.378 16 * * Specification is D&R