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ASTM D4399-05(2023)

(Test Method)

Standard Test Method for Measuring Electrical Conductivity of Electrocoat Baths

Standard Test Method for Measuring Electrical Conductivity of Electrocoat Baths

SIGNIFICANCE AND USE
4.1 The conductivity of electrocoat baths results from the presence of ionic species in the bath, which come from the vehicle and from the presence of impurities present as ionizable acids, bases, salts, or combinations of these. The presence of excessive amounts of ionic impurities is detrimental to the application and performance properties of electrocoating paints. The test is suitable for use in research, production, quality control and electrocoat bath process control.  
4.2 Other related methods for determining the electrical conductivity of water are described in Test Methods D1125.
SCOPE
1.1 This test method covers the determination of the electrical conductivity of electrocoat baths or ultrafiltrate samples using commercially available equipment.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.

General Information

Status
Published
Publication Date
31-May-2023
ICS
25.220.40 - Metallic coatings
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.21 - Chemical Analysis of Paints and Paint Materials
Current Stage
Ref Project

Relations

Refers
ASTM D1193-06 - Standard Specification for Reagent Water
Effective Date
01-Mar-2006
Refers
ASTM D1125-95(2005) - Standard Test Methods for Electrical Conductivity and Resistivity of Water
Effective Date
01-Apr-2005
Refers
ASTM D1125-95(1999) - Standard Test Methods for Electrical Conductivity and Resistivity of Water
Effective Date
10-Jun-1999
Refers
ASTM D1193-99e1 - Standard Specification for Reagent Water
Effective Date
10-Feb-1999
Refers
ASTM D1193-99 - Standard Specification for Reagent Water
Effective Date
10-Feb-1999

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ASTM D4399-05(2023) - Standard Test Method for Measuring Electrical Conductivity of Electrocoat BathsASTM D4399-05(2023) - Standard Test Method for Measuring Electrical Conductivity of Electrocoat Baths
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ASTM D4399-05(2023) - Standard Test Method for Measuring Electrical Conductivity of Electrocoat Baths
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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.
Designation: D4399 − 05 (Reapproved 2023)
Standard Test Method for
Measuring Electrical Conductivity of Electrocoat Baths
This standard is issued under the fixed designation D4399; 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.
1. Scope vehicle and from the presence of impurities present as ioniz-
able acids, bases, salts, or combinations of these. The presence
1.1 This test method covers the determination of the elec-
of excessive amounts of ionic impurities is detrimental to the
trical conductivity of electrocoat baths or ultrafiltrate samples
application and performance properties of electrocoating
using commercially available equipment.
paints. The test is suitable for use in research, production,
1.2 The values stated in SI units are to be regarded as
quality control and electrocoat bath process control.
standard. No other units of measurement are included in this
4.2 Other related methods for determining the electrical
standard.
conductivity of water are described in Test Methods D1125.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Conductivity Bridge—Battery, or AC/DC line-operated,
priate safety, health, and environmental practices and deter-
capable of providing a conductivity reading almost instanta-
mine the applicability of regulatory limitations prior to use.
neously.
1.4 This international standard was developed in accor-
5.2 Conductivity Cell—Dip or fill type, cell constant of 1.0.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5.3 Thermometer—Any type capable of 0.5 °C accuracy
Development of International Standards, Guides and Recom-
with a −2 °C to 32 °C range.
mendations issued by the World Trade Organization Technical
5.4 Measuring Vessel—Any suitable cylindrical container
Barriers to Trade (TBT) Committee.
capable of holding sufficient electrocoat sample to cover the
2. Referenced Documents
electrodes of the conductivity cell, and allowing at least 25 mm
between the conductivity cell and the sides of the vessel.
2.1 ASTM Standards:
D1125 Test Methods for Electrical Conductivity and Resis-
6. Reagents and Materials
tivity of Water
6.1 Purity of Water—References to water shall be under-
D1193 Specification for Reagent Water
stood to mean water conforming to Type II of Specification
3. Summary of Test Method
D1193.
3.1 A specimen is placed in a conductivity cell, or con-
6.2 Cleaning Solvent—An appropriate solvent for the elec-
versely a conductivity cell is placed in an electrocoat material,
trocoat material under measurement.
and the cell is connected to a conductivity bridge. The
electrical conductivity is read directly off the meter of the
7. Sampling and Sample Preparation
bridge as the instantaneous peak reading.
7.1 The sample should be obtained while the electrocoat
4. Significance and Use bath is under proper circulation so that a uniform sample is
obtained. In the case of an ultrafiltrate, the material should be
4.1 The conductivity of electrocoat baths results from the
thoroughly mixed or stirred prior to sampling to ensure
presence of ionic species in the bath, which come from the
uniformity.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
7.2 After sampling and prior to removing a test specimen, it
and Related Coatings, Materials, and Applications and is the direct responsibility of
is mandatory that the samples be shaken or stirred until they are
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
homogeneous and free of any settled material. This is particu-
Current edition approved June 1, 2023. Published June 2023. Originally
larly important if there is a delay between sampling the bath
approved in 1984. Last previous edition approved in 2017 as D4399 – 05 (2017).
DOI: 10.1520/D4399-05R23.
and performing the test on the bath materials. The absence of
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
settled material can be ascertained visually (in a transparent
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
container) or by inserting a spatula, scraping the bottom of the
...

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ABSTRACT
This practice can be used for detection of hexavalent chromium on galvanized and zinc/aluminum alloy coated steel surfaces. Hexavalent chromium-bearing treatments (passivates) can be applied to coated steels to prevent storage stain. Chrome passivation may interfere with the successful pretreatment of galvanized steel, as well as contaminate cleaning and pretreatment baths on a coil coating line. This practice is designed to be a qualitative means of screening chrome passivated coils from those which are not chrome passivated. The following materials will be required to perform the stripping procedure: (1) dark colored or brown polyethylene wash bottle, or brown glass dropper bottle, and (2) test specimens which may be cut panels or coil stock. The following chemical reagents are required to perform this procedure: 1,5-diphenylcarbohydrazide, acetone, ethanol, phosphoric acid, and distilled water. The preparation of indicator solution, procedure of detection, and evaluation of pink color development are detailed. If a material that yields a negative result is suspected of having chromium on the surface, instrumental methods should be used. This technique is not recommended for acrylic resin containing passivation treatments.
SCOPE
1.1 This practice can be used to detect the presence of hexavalent chromium on galvanized and zinc/aluminum alloy coated steel surfaces. Hexavalent chromium-bearing treatments (passivates) can be applied to coated steels to prevent storage stain. While passivated 55 % aluminum-zinc alloy coated steel is commonly painted, passivated galvanized steel is not. Chrome passivation may interfere with the successful pretreatment of galvanized steel, as well as contaminate cleaning and pretreatment baths on a coil coating line.  
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4.1 This practice describes the methods of preparation of hot-dip galvanized surfaces prior to the application of powder coating. The key to achieving proper adhesion between powder coatings and galvanized steel is surface preparation. The surface must be entirely free from visible metal oxides prior to powder coating. Any metal oxides that remain on the surface of the galvanized steel can potentially retain air or moisture. Upon heating during the curing stages of the powder application, the oxides may release water vapor or air, which can expand and penetrate the powder coating, causing blisters or voids.  
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4.1 Different electroplating systems can be corroded under the same conditions for the same length of time. Differences in the average values of the radius or half-width or of penetration into an underlying metal layer are significant measures of the relative corrosion resistance of the systems. Thus, if the pit radii are substantially higher on samples with a given electroplating system, when compared to other systems, a tendency for earlier failure of the former by formation of visible pits is indicated. If penetration into the semi-bright nickel layer is substantially higher, a tendency for earlier failure by corrosion of basis metal is evident.
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4.1 The force required to separate a metallic coating from its plastic substrate is determined by the interaction of several factors: the generic type and quality of the plastic molding compound, the molding process, the process used to prepare the substrate for electroplating, and the thickness and mechanical properties of the metallic coating. By holding all others constant, the effect on the peel strength by a change in any one of the above listed factors may be noted. Routine use of the test in a production operation can detect changes in any of the above listed factors.  
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1.1 This test method gives two procedures for measuring the force required to peel a metallic coating from a plastic substrate.2 One procedure (Procedure A) utilizes a universal testing machine and yields reproducible measurements that can be used in research and development, in quality control and product acceptance, in the description of material and process characteristics, and in communications. The other procedure (Procedure B) utilizes an indicating force instrument that is less accurate and that is sensitive to operator technique. It is suitable for process control use.  
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20.1 This test method covers determination of the total tin in the sample tested and does not apportion the tin to one or the other side of the test specimen. The calculations appearing in Section 27 assume uniform distribution of tin over the two surfaces.  
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SCOPE
1.1 These test methods include four methods for the determination of tin coating weights for electrolytic tin plate as follows:    
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1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
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Standard Test Method for Mechanical Hydrogen Embrittlement Evaluation of Plating/Coating Processes and Service Environments

SIGNIFICANCE AND USE
5.1 Plating/coating Processes—This test method provides a means by which to detect possible hydrogen embrittlement of steel parts during manufacture by verifying strict controls during production operations such as surface preparation, pretreatments, and plating/coating. It is also intended to be used as a qualification test for new plating/coating processes and as a periodic inspection audit for the control of a plating/coating process.  
5.2 Service Environment—This test method provides a means by which to detect possible hydrogen embrittlement of steel parts (plated/coated or bare) due to contact with chemicals during manufacturing, overhaul and service life. The details of testing in a service environment are found in Annex A5.
SCOPE
1.1 This test method describes mechanical test methods and defines acceptance criteria for coating and plating processes that can cause hydrogen embrittlement in steels. Subsequent exposure to chemicals encountered in service environments, such as fluids, cleaning treatments or maintenance chemicals that come in contact with the plated/coated or bare surface of the steel, can also be evaluated.  
1.2 This test method is not intended to measure the relative susceptibility of different steels. The relative susceptibility of different materials to hydrogen embrittlement may be determined in accordance with Test Method F1459 and Test Method F1624.  
1.3 This test method specifies the use of air melted SAE 4340 steel (Grade A, see 7.1.1) per SAE AMS 6415 (formerly SAE AMS-S-5000 and formerly MIL-S-5000) or an alternative VAR (Vacuum Arc Remelt) SAE 4340 steel (Grade B, see 7.1.1) per SAE AMS 6414, and both are heat treated to 260 to 280 ksi (pounds per square inch ×1000) as the baseline. This combination of alloy and heat treat level has been used for many years and a large database has been accumulated in the aerospace industry on its specific response to exposure to a wide variety of maintenance chemicals, or electroplated coatings, or both. Components with ultimate strengths higher than 260 to 280 ksi may not be represented by the baseline. In such cases, the cognizant engineering authority shall determine the need for manufacturing specimens from the specific material and heat treat condition of the component. Deviations from the baseline shall be reported as required by 12.1.2. The sensitivity to hydrogen embrittlement shall be demonstrated for each lot of specimens as specified in 9.5.
Note 1: Extensive testing has shown that VAR 4340 steel may be used as an alternative to the air melted steel with no loss in sensitivity.2
Note 2: VAR 4340 also meets the requirements in AMS 6415 and could be used as an alternative to air melt steel by the steel suppliers because AMS 6415 does not specify a melting practice.  
1.4 Test procedures and acceptance requirements are specified for seven specimens of different sizes, geometries, and loading configurations.  
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1.5.1 The loading conditions and pass/fail requirements for service environments are specified in Annex A5.  
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Standard Practice for Qualitative Adhesion Testing of Metallic Coatings

SIGNIFICANCE AND USE
2.1 These tests are useful for production control and for acceptance testing of products.  
2.2 Interpreting the results of qualitative methods for determining the adhesion of metallic coatings is often a controversial subject. If more than one test is used, failure to pass any one test is considered unsatisfactory. In many instances, the end use of the coated article or its method of fabrication will suggest the technique that best represents functional requirements. For example, an article that is to be subsequently formed would suggest a draw or a bend test; an article that is to be soldered or otherwise exposed to heat would suggest a heat-quench test. If a part requires baking or heat treating after plating, adhesion tests should be carried out after such posttreatment as well.  
2.3 Several of the tests are limited to specific types of coatings, thickness ranges, ductility, or compositions of the substrate. These limitations are noted generally in the test descriptions and are summarized in Table 1 for certain metallic coatings. (A) + Appropriate; − not appropriate.    
2.4 “Perfect” adhesion exists if the bonding between the coating and the substrate is greater than the cohesive strength of either. Such adhesion is usually obtained if good electroplating practices are followed.  
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SCOPE
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