Developed in 1966 by AATCC Commit- heat, sparks and open flame. Use with ad- 6.4 Laboratory gloves (general purpose tee RA56; reaffirmed 1972, 1975, 1978, equate ventilation. Avoid prolonged is sufficient). 1983, 1989; editorially revised 1985, breathing of vapor or contact with skin. 1986, 1990, 1995; revised 1992; edito- Do not take internally. 7. Test Specimens rially revised and reaffirmed 1997. 4.3 Exposure to chemicals used in this Technically equivalent to ISO 14419. procedure must be controlled at or below 7.1 Test two specimens approximately levels set by governmental authorities 20 x 20 cm (8 x 8 in.) from each sample. [e.g., Occupational Safety and Health Condition the test specimens for a mini- 1. Purpose and Scope Administration's (OSHA) permissible mum of 4 hr at 21 ± I C (70 ± 2F) and 65 exposure limits (PEL) as found in 29 ± 2% RH prior to testing. I. I This test method detects the pres- CFR 1910.1000 of January I, 1989]. In ence of a fluorochemical finish, or other addition, the American Conference of 8. Procedure compounds capable of imparting a low Governmental Industrial Hygienists energy surface, on all types offabrics, by (ACGIH) Threshold Limit Values (TLVs) 8.1 Place the test specimen flat on the evaluating the fabric's resistance to wet- comprised of time weighted averages white textile blotting paper on a smooth, ting by a selected series of liquid hydro- (TLV-TWA), short term exposure limits horizontal surface. carbons of different surface tensions. (TLV-STEL) and ceiling limits (TLV-C) 8.1.1 When evaluating open weave of are recommended as a general guide for "thin" fabrics, conduct the test on at least 2. Principle air contaminant exposure which should two layers of the fabric; otherwise, the be met (see 12.1). test liquid may wet the underlying sur- 2.1 Drops of standard test liquids, con- face, not the actual test fabric, and sisting of a selected series of hydrocar- thereby cause confusion in the reading of 5. Uses and limitations bons with varying surface tensions, are the results. placed on the fabric surface and observed 5.1 This test method is not intended to 8.1.2 Equipment, benches and gloves for wetting, wicking, and contact angle. give an absolute measure of the resis- must be free of silicone. Use of silicone The oil repellency grade is the highest tance of the fabric to staining by all oily containing products could adversely af- numbered test liquid which does not wet materials. Other factors, such as compo- fect the oil repellency grade. the fabric surface. sition and viscosity of the oily sub- 8.2 Wearing clean laboratory gloves, stances, fabric construction, fiber type, brush the pile of napped or pile fabrics 3. Terminology dyes, other finishing agents, etc., also in- with your hand in the direction giving the fluence stain resistance. This test can, greatest lay of the surface prior to placing 3.1 grade, n.-in textile testing, the however, provide a rough index of oil the drops ofthe test liquid. symbol for any step of a multistep stan- stain resistance, in that generally the 8.3 Beginning with the lowest-num- dard reference scale for a quality charac- higher the oil repellency grade, the better bered test liquid (AATCC Oil Test Grade teristic. resistance to staining by oily materials, Liquid No. I), care/idly place small drops NOTE: The grade is assigned to test especially liquid oil substances. This is [approximately 5 mm (0.187 in.) in specimens exhibiting a degree of the particularly true when comparing various diameter or 0.05 mL volume] on the test quality comparable to that step of the finishes for a given fabric. specimen in five locations along the fill- standard. ing direction. The drops should be ap- 3.2 oil repellency, n.-in textiles, the 6. Apparatus and Materials proximately 4.0 cm (1.5 in.) apart. The characteristic of a fiber, yarn or fabric dropper tip should be held at a height of whereby it resists wetting by oily liquids. 6.1 Test liquids prepared and num- approximately 0.6 cm (0.25 in.) from the bered according to Table I (see 12.2). fabric surface while placing drops. DO 4. Safety Precautions 6.2 Dropping bottles (see 12.3). NOT TOUCH THE FABRIC WITH 6.3 White AATCC Textile Blotting THE DROPPER T[P. Observe the drops NOTE: These safety precautions are Paper (see 12.4). for 30 ± 2 sec, from approximately a 45° for information purposes only. The pre- angle. cautions are ancillary to the testing proce- 8.4 If no penetration or wetting of the dures and are not intended to be all inclu- fabric at the liquid-fabric interface and no sive. [t is the user's responsibility to use Table I-Standard Test liquids wicking around the drops occur, place safe and proper techniques in handling drops of the next higher-numbered test AATCC Oil materials in this test method. Manufac- Repellency liquid at an adjacent site on the fabric and turers MUST be consulted for specific Grade Number CompOSition again observe for 30 ± 2 sec. details such as material safety data sheets 8.5 Continue this procedure until one and other manufacturer's recommenda- o None (Fails Kaydol) 1 Kaydol of the test liquids shows obvious wetting tions. All OSHA standards and rules or wicking of the fabric under or around 2 65:35 Kaydol: n-hexadecane must also be consulted and followed. by volume the drop within 30 ± 2 sec. 4.1 Good laboratory practices should 3 n-hexadecane be followed. Wear safety glasses and im- 4 n-Ielradecane 9. Evaluation pervious gloves when handling test liq- 5 n-dodecane uids in all laboratory areas. 6 n-decane 9.1 The AATCC Oil Repellency Grade 4.2 The hydrocarbons specified in this 7 n-oclane of a fabric is the numerical value of the method are flammable. Keep away from 8 n-heplane highest-numbered test liquid which will
AATCC Technical Manual/2000 TM 118-1997 191
not wet the fabric within a period of 30 ± fail test liquid. A borderline pass occurs portions of the scale. This interlab in- 2 sec. A grade of zero (0) is assigned if three (or more) of the five drops ap- volved two participants at each of seven when the fabric fails the Kaydol test liq- plied show the rounded drop with partial laboratories rating two specimens of each uid. Wetting of the fabric is normally evi- darkening of the test specimen (Fig. of two fabrics each day for two days. (Day denced by a darkening of the fabric at the 1 [B]). The grade is expressed to the interaction was shown not to be a signifi- liquid-fabric interface or wicking and/or nearest 0.5 value determined by subtract- cant factor in the analysis of the Septem- loss of contact angle of the drop. On black ing one-half from the number of the bor- ber interlab.) Results from both interlabs or dark fabrics, wetting can be detected by derline pass test liquid. were combined for precision and bias loss of "sparkle" within the drop. statements. All materials necessary for the 9.2 Different types of wetting may be 10. Report interlabs were provided to each laboratory encountered depending on the finish, fi- by AATCC including the standard test liq- ber, construction, etc.; and the determina- 10.1 The oil repellency grade should uids. A video cassette of the grading pro- tion of the end point can be difficult on be measured on two separate specimens. cedure prepared at the AATCC Technical certain fabrics. Many fabrics will show If the two grades agree, report the value. Center by the subcommittee and visual complete resistance to wetting by a given When the two grades are not in agree- examples of pass, borderline and fail con- test liquid (as indicated by a clear drop ment, a third determination should be ditions were included in the protocol. The with a high contact angle, see Fig. 1, Ex- made. Report the grade of the third deter- fabrics were limited to polyester/cotton ample A) followed by immediate pene- mination if that value is the same as ei- materials. The unit of measure was the tration by the next higher-numbered test ther of the first two determinations. median of the grades of the two (or three) liquid. In these instances the end point, When the third determination is different specimens rated each day. and oil repellency grade, is obvious. from either ofthe first two, report the me- 11.2 The components of variance as However, some fabrics will show pro- dian value. For example, if the first two standard deviations of the oil repellency gressive wetting under several test liquids grades are 3.0 and 4.0 and the third deter- grade were calculated to be as follows: as evidenced by a partial darkening of the mination is a 4.5 value, report the median AATCC Oil Repellency Test fabric at the liquid-fabric interface (see value of 4.0. Report the oil repellency Fig. 1, Examples B, C and D). For such grade to the nearest 0.5 value (see Fig. 1). Single operator 0.27 fabrics, the point of failure is considered Between operators/ to be that test liquid which exhibits com- within laboratories 0.30 11. Precision and Bias Between laboratories 0.39 plete darkening of the interface or any wicking within 30 ± 2 sec. 11.1 Summary. Interlaboratory tests 11.3 Critical differences. For the com- 9.3 A failure occurs when three (or were conducted in September 1990 and ponents of variance in 11.2, two observa- more) of the five drops applied from a April 1991 to establish the precision of tions should be considered significantly given test liquid show complete wetting this test method. The September interlab different at the 95% probability level if (Fig. 1 [0]) or wicking with loss of con- involved two participants at each of nine the difference equals or exceeds the criti- tact angle (Fig. I [CD. A pass occurs if laboratories rating two specimens of each cal differences shown in Table II. three (or more) of the five drops applied of four fabrics each day for three days. 11.4 Bias. The true value of the oil re- show clear well rounded appearance with The grades of this interlab were concen- pellency grade can only be defined in . high contact angle (Fig. I [AJ). The grade trated into the 1-2 and 4-5 regions of the terms ofthis test method. Within this lim- is expressed as the integer value of the scale. The April interlab was conducted itation, this test method has no known pass test liquid immediately prior to the with fabrics responding in the 2-3 and 5-7 bias.
A = Passes; clear well·rounded drop
B = Borderline pass; rounding drop with partial darkening C = Fails; wicking apparent and/or complete wetting D = Fails; complete wetting
Fig. 1-Grading example.
192 TM 118-1997 AATCC Technical Manual/2000
Table II-Critical Differences' NC 28334; tel: 910/892-8985; fax: 910/892- 12.3 For convenience, it is desirable to 5701; or Textile Innovators Corp., P.O. Box 8, transfer the test liquids from stock solutions to No. of Single Within Between Windsor NC 27983; tel: 252/794-9703; fax: dropping bottles, each marked with the appro- Observalions b Operator laboratory laboratory 252/794-9704. All other hydrocarbon liquids priate AATCC Oil Repellency Grade number. 1 0.75 1.12 1.55 should be laboratory quality available through A typical system found useful consists of 60 most chemical supply houses. One source is mL dropping bottles with ground-in pipettes 2 0.53 0.99 1.45 Fisher Scientific Tnc. That concern's catalog and Neoprene bulbs. Prior to use the bulbs 3 0.43 0.94 1.42 designations are as follows: should be soaked in heptane for several hours and then rinsed in fresh heptane to remove sol- a The critical differences were calculated using t- Specified uble substances. It has been found helpful to 1.950, which is based on infinite degrees of freedom. Melling place the test liquids in sequential order in a b An observation is a unit of measure obtained from Point or wooden platform on the grading table. NOTE: the median of the grades for 2 (or 3) specimens. Catalog Boiling Purity of test liquids does affect surface ten- Test liquid Number Point Range N* sion of the liquid. Use only analytical grades n-hexadecane 03035 17to lBC 27.3 of test liquids. n-tetradecane 04595 4t06C 26.4 12.4 AATCC White Textile Blotting Paper 12. Notes is available from AATCC, P.O. Box 12215, n-dodecane 02666 -10.5 to -9.0C 24.7 12.1 Available from Publications Office, n-decane 0212B 173 to 175C Research Triangle Park NC 27709; tel: 9191 23.5 ACGIH, Kemper Woods Center, 1330 549-8141; fax: 919/549-8933; e-mail: orders@ n-octane 039BO 124to126C 21.4 Kemper Meadow Dr., Cincinnati OH 45240; aatcc.org. n-heptane 0300B 9B to 99C 14.B tel: 513/742-2020. Kaydol 34BC 31.5 12.2 Kaydol™ is available from CBM Group of N.C. Inc., 1308 N. Ellis Ave., Dunn 'N = dynes/em at 25C