ASTM F22-13(2021)
(Test Method)Standard Test Method for Hydrophobic Surface Films by the Water-Break Test
Standard Test Method for Hydrophobic Surface Films by the Water-Break Test
SIGNIFICANCE AND USE
5.1 The water-break test as described in this test method is rapid, nondestructive, and may be used for control and evaluation of processes for the removal of hydrophobic contaminants. This test method is commonly used for in-process verification of the absence of surface contaminants on metal surfaces that may interfere with subsequent surface treatments such as priming, conversion coating, anodizing, plating, or adhesive bonding
5.2 This test method is not quantitative and is typically restricted to applications where a go/no go evaluation of cleanliness will suffice.
5.3 The test may also be used for the detection and control of hydrophobic contaminants in processing environments. For this application, a witness surface free of hydrophobic films is exposed to the environment and subsequently tested. The sensitivity of this test will vary with the level of airborne contaminant and the duration of exposure of the witness surface.
5.4 For quantitative measurement of surface wetting, test methods that measure contact angle of a sessile drop of water or other test liquid may be used in some applications. Measurement methods based on contact angle are shown in Test Methods C813, D5946, and D7490; and Practice D7334.
5.4.1 Devices for in situ measurement of contact angle are available. These devices are limited to a small measurement surface area and may not reflect the cleanliness condition of a larger surface. For larger surface areas, localized contact angle measurement, or other quantitative inspection, combined with water-break testing may be useful.
5.5 For surfaces that cannot be immersed or doused with water, or where such immersion or dousing is impractical, Test Method F21 may be useful.
Note 2: This test method is not appropriate where line of sight evaluation is not feasible; or for assembled hardware where there is a risk for entrapment of water in faying surfaces or complex structures where it may not be effectively removed.
SCOPE
1.1 This test method covers the detection of the presence of hydrophobic (nonwetting) films on surfaces and the presence of hydrophobic organic materials in processing environments. When properly conducted, the test will enable detection of molecular layers of hydrophobic organic contaminants. On very rough or porous surfaces, the sensitivity of the test may be significantly decreased.
1.2 The values stated in SI units are to be regarded as the standard. The inch-pound values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: F22 − 13 (Reapproved 2021)
Standard Test Method for
Hydrophobic Surface Films by the Water-Break Test
ThisstandardisissuedunderthefixeddesignationF22;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope D5946Test Method for Corona-Treated Polymer Films Us-
ing Water Contact Angle Measurements
1.1 This test method covers the detection of the presence of
D7334Practice for Surface Wettability of Coatings, Sub-
hydrophobic (nonwetting) films on surfaces and the presence
strates and Pigments by Advancing Contact Angle Mea-
of hydrophobic organic materials in processing environments.
surement
When properly conducted, the test will enable detection of
D7490TestMethodforMeasurementoftheSurfaceTension
molecular layers of hydrophobic organic contaminants. On
of Solid Coatings, Substrates and Pigments using Contact
veryroughorporoussurfaces,thesensitivityofthetestmaybe
Angle Measurements
significantly decreased.
F21Test Method for Hydrophobic Surface Films by the
1.2 The values stated in SI units are to be regarded as the
Atomizer Test
standard. The inch-pound values given in parentheses are for
information only.
3. Terminology
1.3 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the
3.1.1 contact angle, n—the interior angle that a drop makes
responsibility of the user of this standard to establish appro-
between the substrate and a tangent drawn at the intersection
priate safety, health, and environmental practices and deter-
between the drop and the substrate as shown in Fig. 1; this is
mine the applicability of regulatory limitations prior to use.
theangleformedbyaliquidatthethreephaseboundarywhere
1.4 This international standard was developed in accor-
a liquid, gas (air) and solid intersect.
dance with internationally recognized principles on standard-
3.1.2 hydrophilic—having a strong affinity for water, wet-
ization established in the Decision on Principles for the
table.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
3.1.2.1 Discussion—Hydrophilic surfaces exhibit zero con-
Barriers to Trade (TBT) Committee.
tact angle with water. A sessile drop of water applied to the
surface will immediately spread out to form a film.
2. Referenced Documents
3.1.3 hydrophobic—having little affinity for water, nonwet-
2.1 ASTM Standards:
table.
C813TestMethodforHydrophobicContaminationonGlass
3.1.3.1 Discussion—Hydrophobic surfaces exhibit contact
by Contact Angle Measurement
D351Classification for Natural Muscovite Block Mica and angles between a sessile drop of water and the surface
appreciably greater than zero.
Thins Based on Visual Quality
D1193Specification for Reagent Water 3.1.4 sessile drop—adropofliquidsittingontheupperside
D2578TestMethodforWettingTensionofPolyethyleneand of a horizontal surface.
Polypropylene Films
3.1.5 water-break—a break in the continuity of a film of
water on a surface on removal from an aqueous bath or on
removal of a flowing water source from the surface.
This test method is under the jurisdiction of ASTM Committee E21 on Space
Simulation andApplications of SpaceTechnology and is the direct responsibility of
Subcommittee E21.05 on Contamination.
4. Summary of Test Method
Current edition approved April 1, 2021. Published May 2021. Originally
4.1 The water-break test is performed by withdrawing the
approved in 1962. Last previous edition approved in 2013 as F22–13. DOI:
10.1520/F0022-13R21.
surface to be tested, in a vertical position, from a container of
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
purified water and observing the behavior of the water. For
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
large parts, the test surface may be doused with water and the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. water behavior observed on removal of the water source.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F22 − 13 (2021)
measurement, or other quantitative inspection, combined with
water-break testing may be useful.
5.5 For surfaces that cannot be immersed or doused with
water,orwheresuchimmersionordousingisimpractical,Test
Method F21 may be useful.
NOTE 2—This test method is not appropriate where line of sight
evaluation is not feasible; or for assembled hardware where there is a risk
A = contact angle
for entrapment of water in faying surfaces or complex structures where it
D=dropofliquid
may not be effectively removed.
P = specimen
T = tangent at specimen surface
6. Interferences
FIG. 1 Contact Angle
6.1 Loss of sensitivity may result from either of the follow-
ing factors:
6.1.1 The presence of hydrophilic substances on the surface
4.2 Theinterpretationofthetestisbaseduponthepatternof
to be tested, in the test equipment, or in the test materials, or
wetting. Contaminated areas having a surface tension lower
6.1.2 An unusually rough or porous surface condition.
than water will cause the water to bead up at that location or
6.2 On hot parts or in elevated temperature conditions,
“break” while draining. Most common film contaminants such
asoils,silicones,orfluorocarbongreaseshavesurfacetensions water may evaporate before water-break can be observed.
significantly lower than water. In the absence of hydrophobic
7. Apparatus
films, the draining water layer will remain as a film over the
surface. In areas where hydrophobic materials are present on
7.1 Overflow Container, such as a glass beaker for small
the surface, the draining water layer will break up into a
parts.
discontinuous film within one minute.
7.2 Purified Water Source, final rinse tank or dousing hose
NOTE 1—It is possible to use this test method with liquids other than
and drain, for large parts.
water.Liquidswithdifferentwettingtensionswillexhibitdifferentcontact
angles with a given surface and therefore different levels of sensitivity to
7.3 Low Power Microscope, (5 to 50×) and light source for
hydrophobic films. This principle has been applied to develop differential
observation of small piece parts (optional).
wetting tension tests such as described in Test Method D2578 using
standardized liquids commonly referred to as dyne liquids.
8. Reagents and Materials
5. Significance and Use
8.1 Purity of Water—DeionizedordistilledwaterperSpeci-
ficationD1193TypesII,III,orIVispreferred.Waterofhigher
5.1 The water-break test as described in this test method is
ionic content may render the test destructive. The water used
rapid, nondestructive, and may be used for control and evalu-
must be free of hydrophobic and hydrophilic substances.When
ation of processes for the removal of hydrophobic contami-
processing large parts in a production environment, the water
nants. This test method is commonly used for in-process
shall be sampled directly from the rinse tank or at the exit of
verification of the absence of surface contaminants on metal
thedousingwatersourcepriortowater-breaktest.Hydrophilic
surfaces that may interfere with subsequent surface treatments
contaminantssuchastracesurfactantspresentontherinsetank
such as priming, conversion coating, anodizing, plating,
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: F22 − 13 F22 − 13 (Reapproved 2021)
Standard Test Method for
Hydrophobic Surface Films by the Water-Break Test
This standard is issued under the fixed designation F22; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
1.1 This test method covers the detection of the presence of hydrophobic (nonwetting) films on surfaces and the presence of
hydrophobic organic materials in processing environments. When properly conducted, the test will enable detection of molecular
layers of hydrophobic organic contaminants. On very rough or porous surfaces, the sensitivity of the test may be significantly
decreased.
1.2 The values stated in SI units are to be regarded as the standard. The inch-pound values given in parentheses are for information
only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
C813 Test Method for Hydrophobic Contamination on Glass by Contact Angle Measurement
D351 Classification for Natural Muscovite Block Mica and Thins Based on Visual Quality
D1193 Specification for Reagent Water
D2578 Test Method for Wetting Tension of Polyethylene and Polypropylene Films
D5946 Test Method for Corona-Treated Polymer Films Using Water Contact Angle Measurements
D7334 Practice for Surface Wettability of Coatings, Substrates and Pigments by Advancing Contact Angle Measurement
D7490 Test Method for Measurement of the Surface Tension of Solid Coatings, Substrates and Pigments using Contact Angle
Measurements
F21 Test Method for Hydrophobic Surface Films by the Atomizer Test
3. Terminology
3.1 Definitions:
This test method is under the jurisdiction of ASTM Committee E21 on Space Simulation and Applications of Space Technology and is the direct responsibility of
Subcommittee E21.05 on Contamination.
Current edition approved Nov. 1, 2013April 1, 2021. Published November 2013May 2021. Originally approved in 1962. Last previous edition approved in 20072013 as
F22 – 02 (2007).F22 – 13. DOI: 10.1520/F0022-13.10.1520/F0022-13R21.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F22 − 13 (2021)
3.1.1 contact angle, n—the interior angle that a drop makes between the substrate and a tangent drawn at the intersection between
the drop and the substrate as shown in Fig. 1; this is the angle formed by a liquid at the three phase boundary where a liquid, gas
(air) and solid intersect.
3.1.2 hydrophilic—having a strong affinity for water, wettable.
3.1.2.1 Discussion—
Hydrophilic surfaces exhibit zero contact angle with water. A sessile drop of water applied to the surface will immediately spread
out to form a film.
3.1.3 hydrophobic—having little affinity for water, nonwettable.
3.1.3.1 Discussion—
Hydrophobic surfaces exhibit contact angles between a sessile drop of water and the surface appreciably greater than zero.
3.1.4 sessile drop—a drop of liquid sitting on the upper side of a horizontal surface.
3.1.5 water-break—a break in the continuity of a film of water on a surface on removal from an aqueous bath or on removal of
a flowing water source from the surface.
4. Summary of Test Method
4.1 The water-break test is performed by withdrawing the surface to be tested, in a vertical position, from a container of purified
water and observing the behavior of the water. For large parts, the test surface may be doused with water and the water behavior
observed on removal of the water source.
4.2 The interpretation of the test is based upon the pattern of wetting. Contaminated areas having a surface tension lower than
water will cause the water to bead up at that location or “break” while draining. Most common film contaminants such as oils,
silicones, or fluorocarbon greases have surface tensions significantly lower than water. In the absence of hydrophobic films, the
draining water layer will remain as a film over the surface. In areas where hydrophobic materials are present on the surface, the
draining water layer will break up into a discontinuous film within one minute.
NOTE 1—It is possible to use this test method with liquids other than water. Liquids with different wetting tensions will exhibit different contact angles
with a given surface and therefore different levels of sensitivity to hydrophobic films. This principle has been applied to develop differential wetting
tension tests such as described in Test Method D2578 using standardized liquids commonly referred to as dyne liquids.
5. Significance and Use
5.1 The water-break test as described in this test method is rapid, nondestructive, and may be used for control and evaluation of
processes for the removal of hydrophobic contaminants. This test method is commonly used for in-process verification of the
absence of surface contaminants on metal surfaces that may interfere with subsequent surface treatments such as priming,
conversion coating, anodizing, plating, or adhesive bonding
5.2 This test method is not quantitative and is typically restricted to applications where a go/no go evaluation of cleanliness will
suffice.
A = contact angle
D = drop of liquid
P = specimen
T = tangent at specimen surface
FIG. 1 Contact Angle
F22 − 13 (2021)
5.3 The test may also be used for the detection and control of hydrophobic contaminants in processing environments. For this
application, a witness surface free of hydrophobic films is exposed to the environment and subsequently tested. The sensitivity of
this test will vary with the level of airborne contaminant and the duration of exposure of the witness surface.
5.4 For quantitative measurement of surface wetting, test methods that measure contact angle of a sessile drop of water or other
test liquid may be used in some applications. Measurement methods based on contact angle are shown in Test Methods C813,
D5946, and D7490; and Practice D7334.
5.4.1 Devices for in situ measurement of contact angle are available. These devices are limited to a small measurement surface
area and may not reflect the cleanliness condition of a larger surface. For larger surface areas, localized contact angle measurement,
or other quantitative inspection, combined with water-break testing may be useful.
5.5 For surfaces that cannot be immersed or doused with water, or where such immersion or dousing is impractical, Test Method
F21 may be useful.
NOTE 2—This test method is not appropriate where line of sight evaluation is not feasible; or for asse
...
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