AATC C Technical Manual/2014
TM 118-2013207
Developed in 1966 by AATCC Committee RA56; reaffirmed 1972, 1975, 1978,1983, 1989, 2002, 2012; editorially re-vised 1985, 1986, 1990, 1995, 2004,2008, 2010; revised 1992, 2007, 2013;editorially revised and reaffirmed 1997.Technically equivalent to ISO 14419.
1. Purpose and Scope
1.1 This test method is used to detect the presence of a fluorochemical finish,or other compounds capable of imparting a low energy surface, on all types of fab-rics, by evaluating the fabric’s resistance to wetting using a selected series of liquid hydrocarbons of different surface tensions.
2. Principle
2.1 Drops of standard test liquids, con-sisting of a selected series of hydrocar-bons with varying surface tensions, are placed on the fabric surface and observed for wetting, wicking and contact angle.The oil repellency grade is the highest numbered test liquid which does not wet the fabric surface.
3. Terminology
3.1 grade, n.—in textile testing , the symbol for any step of a multistep stan-dard reference scale for a quality charac-teristic.
NOTE: The grade is assigned to test specimens exhibiting a degree of the quality comparable to that step of the standard.
3.2 oil repellency, n.—in textiles , the characteristic of a fiber, yarn or fabric whereby it resists wetting by oily liquids.
4. Safety Precautions
NOTE: These safety precautions are for information purposes only. The pre-cautions are ancillary to the testing proce-dures and are not intended to be all inclu-sive. It is the user’s responsibility to use safe and proper techniques in handling materials in this test method. Manufac-turers MUST be consulted for specific details such as material safety data sheets and other manufacturer’s recommenda-tions. All OSHA standards and rules must also be consulted and followed.4.1 Good laboratory practices should be followed. Wear safety glasses and im-pervious gloves when handling test liq-uids in all laboratory areas.
4.2 The hydrocarbons specified in this method are flammable. Keep away from
heat, sparks and open flame. Use with ad-equate ventilation. Avoid prolonged breathing of vapor or contact with skin.Do not take internally.
4.3 Exposure to chemicals used in this procedure must be controlled at or below levels set by governmental authorities [e.g., Occupational Safety and Health Administration’s (OSHA) permissible ex-posure limits (PEL) as found in 29 CFR 1910.1000; see web site: v for latest version]. In addition, the Ameri-can Conference of Governmental Indus-trial Hygienists (ACGIH) Threshold Limit V alues (TLVs) comprised of time weighted averages (TLV-TWA), short term exposure limits (TLV-STEL) and ceiling limits (TLV-C) are recommended as a general guide for air contaminant ex-posure which should be met (see 12.1).
5. Uses and Limitations
5.1 This test method is not intended to give an absolute measure of the resis-tance of the fabric to staining by all oily materials. Other factors, such as compo-sition and viscosity of the oily sub-stances, fabric construction, fiber type,dyes, other finishing agents, etc., also in-fluence stain resistance. This test can,however, provide a rough index of oil stain resistance, in that generally the higher the oil repellency grade, the better resistance to staining by oily materials,especially liquid oil substances. This is particularly true when comparing various finishes for a given fabric.
6. Apparatus and Materials (see 12.2)
6.1 Test liquids prepared and num-bered according to Table I (see 12.3, 12.4and 12.5).
6.2 Dropping bottles (see 12.4).
6.3 White AATCC Textile Blotting Paper (see 12.6).
6.4 Laboratory gloves (general purpose is sufficient).
7. Test Specimens
7.1 Test two specimens of the same size from each sample. Specimen size should be sufficient to allow for the com-plete range of test liquids to be evaluated,but shall be no smaller than 20 × 20 cm (8× 8 in.) and no larger than 20 × 40 cm (8× 16 in.). Specimens from sample to sam-ple should be the same size. Condition the test specimens for a minimum of 4 h at 21 ± 1°C (70 ± 2°F) and 65 ± 2% RH prior to testing (see 12.7).
8. Procedure
8.1 Place the test specimen flat on the white textile blotting paper on a smooth,horizontal surface.
8.1.1 When evaluating open weave of “thin” fabrics, conduct the test on at least two layers of the fabric; otherwise, the test liquid may wet the underlying sur-face, not the actual test fabric, and thereby cause confusion in the reading of the results.
8.1.2 Equipment, benches and gloves must be free of silicone. Use of silicone containing products could adversely af-fect the oil repellency grade.
8.2 Wearing clean laboratory gloves,brush the pile of napped or pile fabrics with your hand in the direction giving the greatest lay of the surface prior to placing the drops of the test liquid.
8.3 Beginning with the lowest-num-bered test liquid (AATCC Oil Test Grade Liquid No. 1), carefully place small drops [approximately 5 mm (0.187 in.) in diameter or 0.05 mL volume] on the test specimen in five locations along the fill-ing direction. The drops should be ap-proximately 4.0 cm (1.5 in.) apart. The dropper tip should be held at a height of approximately 0.6 cm (0.25 in.) from the fabric surface while placing drops. DO NOT TOUCH THE FABRIC WITH THE DROPPER TIP. Observe the drops for 30± 2 s, from approximately a 45° angle.8.4 If no penetration or wetting of the fabric at the liquid-fabric interface and no wicking around the drops occur, place drops of the next higher-numbered test liquid at an adjacent site on the fabric and again observe for 30 ± 2 s.
8.5 Continue this procedure until one of the test liquids shows obvious wetting or wicking of the fabric under or around the drop within 30 ± 2 s.
AATCC Test Method 118-2013
Oil Repellency: Hydrocarbon Resistance Test
Table I—Standard Test Liquids
AATCC Oil Repellency Grade Number
Composition
0None (Fails Mineral Oil)1Mineral Oil
265:35 Mineral Oil:
n-hexadecane by volume 3n-hexadecane 4n-tetradecane 5n-dodecane 6n-decane 7n-octane 8
n-heptane
Copyright © 2013 American Association of Textile Chemists and Colorists
208TM 118-2013
AATC C Technical Manual/2014
9. Evaluation
9.1 The AA TCC Oil Repellency Grade of a fabric is the numerical value of the highest-numbered test liquid which will not wet the fabric within a period of 30 ±2 s. A grade of zero (0) is assigned when the fabric fails the mineral oil test liquid.Wetting of the fabric is normally evi-denced by a darkening of the fabric at the liquid-fabric interface or wicking and/or loss of contact angle of the drop. On black or dark fabrics, wetting can be detected by loss of “sparkle” within the drop.
9.2 Different types of wetting may be encountered depending on the finish, fi-ber, construction, etc.; and the determina-tion of the end point can be difficult on certain fabrics. Many fabrics will show complete resistance to wetting by a given test liquid (as indicated by a clear drop with a high contact angle, see Fig. 1, Ex-ample A) followed by immediate pene-tration by the next higher-numbered test liquid. In these instances the end point,and oil repellency grade, is obvious.However, some fabrics will show pro-gressive wetting under several test liquids as evidenced by a partial darkening of the fabric at the liquid-fabric interface (see Fig. 1, Examples B, C and D). For such fabrics, the point of failure is c
onsidered to be that test liquid which exhibits com-plete darkening of the interface or any wicking within 30 ± 2 s.
9.3 A failure occurs when three (or more) of the five drops applied from a given test liquid show complete wetting (Fig. 1[D]) or wicking with loss of con-tact angle (Fig. 1[C]). A pass occurs if three (or more) of the five drops applied
show clear well rounded appearance with high contact angle (Fig. 1[A]). The grade is expressed as the integer value of the pass test liquid immediately prior to the fail test liquid. A borderline pass occurs if three (or more) of the five drops ap-plied show the rounded drop with partial darkening of the test specimen (Fig.1[B]). The grade is expressed to the nearest 0.5 value determined by subtract-ing one-half from the number of the bor-derline pass test liquid.
10. Report
10.1 The specimen size used for testing should be reported (see 7.1).
10.2 The oil repellency grade should be measured on two separate specimens.If the two grades agree, report the value.When the two grades are not in agree-ment, a third determination should be made. Re
port the grade of the third deter-mination if that value is the same as ei-ther of the first two determinations.When the third determination is different from either of the first two, report the me-dian value. For example, if the first two grades are 3.0 and 4.0 and the third deter-mination is a 4.5 value, report the median value of 4.0. Report the oil repellency grade to the nearest 0.5 value (see Fig. 1).
11. Precision and Bias
11.1 Summary . Interlaboratory tests were conducted in September 1990 and April 1991 to establish the precision of this test method. The September interlab involved two participants at each of nine laboratories rating two specimens of each of four fabrics each day for three days.The grades of this interlab were concen-trated into the 1-2 and 4-5 regions of the scale. The April interlab was conducted with fabrics responding in the 2-3 and 5-7portions of the scale. This interlab in-volved two participants at each of seven laboratories rating two specimens of each of two fabrics each day for two days. (Day interaction was shown not to be a signifi-cant factor in the analysis of the Septem-ber interlab.) Results from both interlabs were combined for precision and bias statements. All materials necessary for the interlabs were provided to each laboratory by AA TCC including the standard test liq-uids. A video cassette of the grading pro-cedure prepared at the AA TCC Technical Center by the subcommittee and visual examples of pass, borderline and fail con-ditions were included in the protocol. The fabrics were
limited to polyester/cotton materials. The unit of measure was the median of the grades of the two (or three)specimens rated each day.
11.2 The components of variance as standard deviations of the oil repellency grade were calculated to be as follows:
AATCC Oil Repellency Test
Single operator 0.27Between operators/within laboratories 0.30Between laboratories
0.39
11.3 Critical differences . For the com-ponents of variance in 11.2, two observa-tions should be considered significantly different at the 95% probability level if the difference equals or exceeds the criti-cal differences shown in Table II.
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.
Copyright © 2013 American Association of Textile Chemists and Colorists
AATC C Technical Manual/2014
TM 118-2013209
editorially11.4 Bias . The true value of the oil re-pellency grade can only be defined in terms of this test method. Within this limi-tation, this test method has no known bias.
12. Notes
12.1 Available from Publications Office,ACGIH, Kemper Woods Center, 1330 Kemper Meadow Dr., Cincinnati OH 45240; tel: +1.513.742.2020; web site:
12.2 For potential equipment information pertaining to this test method, please visit the online AATCC Buyer’s Guide at /bg. AATCC provides the pos-
sibility of listing equipment and materials sold by its Corporate members, but AATCC does not qualify, or in any way approve, endorse or certify that any of the listed equipment or materials meets the requirements in its test methods.
12.3 Standard test liquid information listed below:
12.4 For convenience, it is desirable to transfer the test liquids from stock solutions to dropping bottles, each marked with the appro-priate AATCC Oil Repellency Grade number.A typical system found useful consists of 60mL dropping bottles with ground-in pipettes
Test Liquid Specified Melting Point or Boiling Point
Range
N*
n-hexadecane 17-18°C 27.3n-tetradecane 4-6°C 26.4n-dodecane –10.5-–9.0°C 24.7n-decane 173-175°C 23.5n-octane 124-126°C 21.4n-heptane 98-99°C 19.8Mineral Oil 174-177°C 31.5
*N = dynes/cm at 25°C
and Neoprene bulbs. Prior to use the bulbs should be soaked in heptane for several hours and then rinsed in fresh heptane to remove sol-uble substances. It has been found helpful to place the test liquids in sequential order in a wooden platform on the grading table. NOTE:Purity of test liquids does affect surface ten-sion of the liquid. Use only analytical grades of test liquids.
12.5 Mineral oil, for the purpose of this test,is defined as the commercial product com-monly known as White Mineral Oil, USP,Food Grade or better, CAS #8012-95-1, with a Saybolt viscosity at 38°C (100°F) between 340-360. Boiling Point between 174-177°C (346-350°F), Specific Gravity between 0.840-0.890; and Flash Point greater than 188°C (370°F); Kaydol ™ and Crystal Plus ™ are two well k
nown trade names in the United States;other brands may be suitable.
12.6 Available from AATCC, P.O. Box 12215, Research Triangle Park NC 27709; tel:+1.919.549.8141; fax: +1.919.549.8933; e-mail: ; web site:
12.7 Often AATCC Methods 193 (Aqueous Liquid Repellency: Water/Alcohol Solution Resistance) and 118 are done concurrently. It is recommended that the specimen sizes for each test be the same.
Table II—Critical Differences a
No. of Observations b Single Operator Within Laboratory Between Laboratory
10.75 1.12 1.5520.530.99 1.453
0.430.94 1.42
a
The critical differences were calculated using t -1.950, which is based on infinite degrees of freedom.b
An observation is a unit of measure obtained from the median of the grades for 2 (or 3) specimens.
Copyright © 2013 American Association of Textile Chemists and Colorists
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