LUBRIZOL STANDARD TEST PROCEDURE

TEST PROCEDURE AATM 516-01 Edition: October 13, 2006 Previous Edition: November 30, 1999

PEROXIDE VALUE - AOCS METHOD

APPARATUS 1. 2. 3. 4. 5. 6. Balance capable of weighing to the nearest 0.1 mg. 250 ml. glass stoppered Erlenmeyer flasks. 10 ml Class B Burette, graduated in 0.05 divisions, with a tolerance of 0.04 ml. Mohr pipette capable of containing 1 ml with a tolerance of 0.04 ml. 2-graduated cylinders capable of containing 50 ml. Dispensing device, capable of dispensing 1 ml.

REAGENTS AND SOLUTIONS 1. 2. 3. 4. 5. Acetic Acid - chloroform solution (480ml Acetic Acid and 320ml Chloroform). Saturated Potassium Iodide solution. Store in the dark. Sodium thiosulfate solution, 0.1N. Commercially available. 1% Starch solution. Commercially available. Distilled or deionized water.

PROCEDURE Conduct a blank determination of the reagents daily. 1. Weigh 5.00 (0.05)g of sample into a 250 ml glass stoppered Erlenmeyer flask. Record weight to the nearest 0.01g. By graduated cylinder, add 30 ml of the acetic acid - chloroform solution. Swirl the flask until the sample is completely dissolved (careful warming on a hot plate may be necessary).

2. 3.

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2 PROCEDURE cont. 4. 5. 6. Using 1 ml Mohr pipette, add 0.5 ml of saturated potassium iodide solution. Stopper the flask and swirl the contents of the flask for exactly one minute. Immediately add by graduated cylinder, 30 ml of either distilled or deionized water, stopper and shake vigorously to liberate the iodine from the chloroform layer. Fill the burette with 0.1N sodium thiosulfate. If the starting color of the solution is deep red orange, titrate slowly with mixing until the color lightens. If the solution is initially a light amber color, go to step 9. Using a dispensing device, add 1 ml of starch solution as indicator.

7. 8.

9.

10. Titrate until the blue gray color disappears in the aqueous (upper layer). Note: for Doe-120, titrate until the lower layer has a "milky" appearance. 11. Accurately record the mls of titrant used to two decimal places.

CALCULATIONS S = titration of sample B= titration of blank Peroxide value = (S - B) X N thiosulfate X weight of sample or (S - B) X N thiosulfate X 200 1000

PRECISION* Product DOE-120 Average 4.12 Std. Dev. 1.04 Coeff. of Var. 25.11 Df 10 Cm **

*Data from Institute WV Project Report 7-24-98