How-SNP-Tests_Oil-and-Grease-Resistance.pptx
- 1. Oil and Grease Resistance Test Methods SNP Inc.
- 2. Most common OGR test methods • 3M® Kit Test (Tappi T559) • Turpentine Test (Tappi T454) • Permeability Test (ISO 16532-1)
- 3. 3M® Kit Test • Well-known by paper and board manufacturers and suppliers • Measures the degree of repellency of paper or boards treated with fluorochemical sizing agents • Used to quantify and compare performance of cellulose substrates used for food contact and other packaging applications • Easy, cheap, quick and reproducible
- 4. Turpentine Test • Utilizes silica sand in conjunction with dyed turpentine • Time taken for dye to penetrate substrate is then determined • Not always the most suitable method for assessment of cellulose substrates having grease or oil resistance through use of coating or internal treatment
- 5. Permeability Test • Determines the grease resistance of both creased and uncreased cellulose substrates by determination of time taken for palm kernel oil (a simulated fat material) to penetrate into fibers • Method is equally applicable to cellulose substrates that have been internally or surface sized with organophobic materials, or plastic coatings
- 6. Comparison of OGR Testing Methods Test Method Test Description Test substance Test Conditions 3M Kit Test (TAPPI T-55 pm-96) Paper surface tension checked by applying a series of test solutions Mixtures of castor oil, toluene, n- heptane RT, 15 seconds Turpentine Test (TAPPI T-454 om-89) Stained Turpentine Spirit/Sand mixture applied on paper and time to penetration recorded Turpentine Spirit RT, 30 minutes Permeability Test (ISO 16532-1) Oil applied to creased and uncreased paper and time to penetration recorded Palm Kernel Oil 110°C, 20 minutes Hot Mazola Oil Test Hot Oil applied on paper and staining and % adsorption recorded Corn Oil 110°C, 20 minutes Oleic Acid Test Staining, pin holes checked by applying a series of test solutions Mixtures of castor oil, oleic acid and octanoic acid 60°C, 6 minutes RP-2 Test Stained RP Oil/Sand applied and % staining recorded RP proprietary oil 60°C, 24 hours Pet-Food Test Pet-food pellets applied under pressure and % staining recorded Pet-food pellets 60-70°C, 16 hours-7 days Fatty Acid Test Staining checked by applying a series of test solutions Mixtures of free fatty acids of different carbon chain lengths 60°C, 10 minutes
- 7. 3M® Kit Test Solution Compositions Value Castor Oil (% vol.) Toluene (% vol.) n-Heptane (% vol.) Surface Tension (dynes/cm) 1 100 0 0 33.9 2 90 5 5 31.2 3 80 10 10 28.8 4 70 15 15 27.6 5 60 20 20 26.3 6 50 25 25 25.3 7 40 30 30 24.8 8 30 35 35 24.4 9 20 40 40 24.1 10 10 45 45 24.0 11 0 50 50 23.8 12 0 45 55 23.4
- 8. Surface Tensions of 3M® Kit Test Solutions Kit Value Surface Tension (dynes/cm) 1 33.9 2 31.2 3 28.8 4 27.6 5 26.3 6 25.3 7 24.8 8 24.4 9 24.1 10 24.0 11 23.8 12 23.4 Wetting of surfaces by liquid is ruled by surface tesnion of liquid vs. surface energy of solid Liquid = contact angle Solid surface S = surface energy of solid L = surface tension liquid Liquid wets completely solid if L < S
- 9. 3M® Kit Test FAIL PASS #1 #2 #3 #4 #5 #5 #5 #5 • Passed #4, failed at #5. Kit Value =#4.
- 10. Problem with Kit Test Use to Predict OGR Performance in Use • It does not always correlate with in-use performance due to the presence of solvents in test solutions • Coatings providing good oil and grease resistance but poor solvent resistance will fail therefore not accurately predicting in-performance use • Does not account for hydrostatic pressure exerted by packaged goods • In-use performance of non-fluorochemical containing coatings and papers can not be predicted by this test method • Foods do not contain solvent
- 11. 1. Prepare colored turpentine test fluid by adding 5 grams of anhydrous calcium chloride and 1.0 gram of a suitable oil- soluble red dye to 100 grams of turpentine in a capped bottle. 2. Shake well and let stand for at lease 6 hours, shaking occasionally. 3. Warm solution to approximately 70 deg F. 4. Filter solution through a dry filter paper. 5. Place back in air tight capped bottle. Preparation of Turpentine Test Solution
- 12. Turpentine Test Procedure 1. Using a pencil, mark a 72 x 72 inch square on the treated side of the specimen to be tested. The specimen should be free of creases or folds and should be placed a smooth flat surface. 2. Using a stencil brush apply the turpentine test solution to the specimen. 3. Start timer and time 60 seconds. 4. Wipe surface and count # of pinholes present. Test at least 6 specimens and report maximum and minimum of pinholes observed.
- 13. Permeability Test-TAPPI T-507 Pressure block 720g Oil Indicator The prepared paper 100mm x 100mm Saturated blotting paper 75mmx75mm Clean blotting paper 100mm x 100mm Aluminum foil 100mm x 100mm Pressure block 720g
- 14. Hot Mazola Test Procedure 1. Weigh specimen on balance with accuracy of 0.001g or better. 2. Set-up and test as if running a Cobb test (TAPPI T- 441), except replace water with corn oil. 3. Place specimen in a 110 degree C oven for 20 minutes. 4. After 20 minutes, remove from oven and pour off oil. 5. Remove specimen from Cobb tester. 6. Place two standard blotter sheets over specimen and remove excess oil by moving a roller having a smooth face 20 cm wide and weighing 10.0 ± 0.5 kg (22 ± 1.1 lb) over its surface. 7. Reweight the specimen and calculate the amount oil absorbed/unit area of the test specimen. **Note if staining is observed. If oil penetrates specimen mark as failed.
- 15. Oleic Acid Test Solution Compositions Test Composition (%w) Solution # %Castor Oil %Oleic Acid %Octanoic Acid 1 100 0 0 2 50 50 0 3 30 70 0 4 0 100 0 5 0 80 20 6 0 70 30 7 0 55 45 8 0 35 65 9 0 20 80 10 0 10 90 11 0 0 100
- 16. Procedure 1. Place specimen inside a preheated 60 degree oven on a flat surface with side to be tested facing up. 2. Without touching dropper to the surface of the paper, place one drop of each test solution onto the surface of the paper. Drop height should be 1-2 cm. 3. Close the oven and start timer. 4. After 6 min, remove sample from oven and wipe excess reagent from the surface with an absorbent material. 5. Evaluate the surface of the sample at each drop placement area and note if penetration, dark staining, or pinholes are observed. 6. Record highest # reagent that did not cause failure (penetration). 7. Record highest reagent# for which no visual staining was observed. 8. Report presence of pinholes as “Yes” or “No”.
- 17. RP-2 OGR Performance Test • Store at 60 C for 24 hrs. • Report stained squares as percent failure. Red stained RP synthetic oil (Ralston-Purina proprietary) Ottawa sand (5g, 20-30 mesh) Treated paper sample (Creased on diagonals) Grid printed sheet (10x10cm)
- 18. Pet Food Performance Test Conditions: Temp. = 60-70 °C R.H. = 50-65% Duration = 16-24 hours Report results as % stained surface
- 19. Surface tension (dynes/cm) 31-32 Cooking oil (2) 40 - 50 Untreated paper (1) 27-28 Free fatty acids (2) 6 CF3 monolayer (3) 18 -CF2- sequence (PTFE) (3) Natural fats and oils Ideal CF2 coverage Ideal CF3 coverage Values detected at 20°C Source: (1) Borch J., J. Adhesion Sci. Technol., 5(7), 523 (1991(; (2) Solvay Solexis internal data (3) Zisman W.A., Contact Angle, Wettability and Adhesion, Advances in Chemistry Series, Vol 43 (1964) and refs. teherein Surface tension values of liquids and surfaces
- 20. Paper Wetting Mechanisms by Oils/Fats
- 21. Low polarity/Low reactivity R = C6 to C22 Polarity/Reactive groups Fats/Oils Chemical Structure
- 22. A) Non-polar, non-reactive oils - surface energy of treated paper vs. liquid surface tension - solubility effects - capillary adsorption contribution B) Reactive, polar oils - polar interaction with paper constituents *Both mechanisms need to be considered when formulating a coating to meet application requirements Parameters Affecting Oil Adsorption
- 23. Type of fatty acid Oil or Fat 4:0 6:0 8:0 10:0 12:0 14:0 16:0 18:0 20:0 16:1 18:1 20:1 18:2 18:3 SoybeanOil 11 4 24 54 7 Corn Oil 11 2 28 58 1 Cottonseed Oil 1 22 3 1 19 54 1 Palm Oil 1 45 4 40 10 Peanut Oil (1) 11 2 1 48 2 32 Olive Oil 13 3 1 1 71 10 1 Canola Oil 4 2 62 22 10 Safflower Oil 7 2 13 78 Sunflower Oil 7 5 19 68 1 Mid Oleic Sunflower oil 4 5 65 26 Coconut Oil 1 8 6 47 18 9 3 6 2 Palm kernel oil 3 4 48 16 8 3 15 2 Cocoa butter 26 34 1 34 3 Butterfat (2) 4 2 1 3 3 11 27 12 2 29 2 1 Chicken fat 1 25 8 5 45 15 1 Lard 2 26 14 3 44 1 10 Beef tallow (3) 3 24 19 4 43 3 1 (1) Peanut oil typically contains C22:0 plus C24:0 at 4-5% of total fatty acids (2) Butterfat typically contains C15:0 plus C17:0 at about 3% of total fatty acids (3) Beef tallow typically contains C15:0 plus C17:0 at about 2% and C14:1 plus C17:1 at about 2% of total fatty acids • Fatty acid composition of natural oils and fats (contained as tryglicerides) Oils and Fats Composition
- 24. How do different carbon chain lengths in Free Fatty Acids (FFA) affect penetration? 1. Penetration through the coated substrate is related to the carbon chain length. 2. The greater the number of lower carbon chain free fatty acids will result in more aggressive penetration of FFA. Fatty Acids Penetration
- 25. Free Fatty Acids in Packed Materials Pet Foods > Generally containing from 10 to 27% crude fat > Crude fat contains 10 to 30% FFAs by weight > FFAs in pet-food materials can range from 1 to 9% Butter > W/O emulsions > Triglycerides hydrolysis takes place Chicken Fat > May contain up to 10% FFA
- 26. FFA Alternative to Kit Test
- 27. • Test fluids increase in aggressiveness as percent of shorter chain FFA increase • Unlike kit solutions, there is little variation in surface tension of fluids over time Test Solutions: 5 Fatty Acids Mixtures Components Mixture A (Diluted Oleic acid) (% wt.) Mixture B (Olive Oil fatty acids) (% wt.) Mixture C (Beef tallow fatty acids) (% wt.) Mixture D (Butterfat fatty acids) (% wt.) Mixture E (Coconut oil fatty acids) (% wt.) Castor Oil 80 - - - - Oleic - C18:1 20 75 62 41 9 Linoleic - C18:2 - 11 4 3 2 Palmitic – C16:0 - 14 32 38 18 Lauric - C12:0 - - 2 8 56 Capric - C10:0 - - - 3 6 Caprylic - C8:0 1 8 Caproic - C6:0 6 1 Surface Tension (dynes/cm) 31.5 28.2 28.1 27.4 26.7
- 28. 1. Test fluids are more reflective of what will be seen in use. 2. Test fluids contain no solvents. 3. Temperature of 60C can be used to accelerate test results. 4. Test fluids are stable over time. Benefits of Test Method
- 29. 1. Apply test fluids in same manner as kit solutions. 2. Keep mixtures in oven at 60°C prior to use. 3. Place sample with test fluieds in oven at 60°C for 10 minutes. 4. Remove from oven and observe staining. 5. Paper is rated with the # of highest mixture that does not stain. Fatty Acid Test Procedure Fail Pass