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: B733 − 22

Standard Specification for

Autocatalytic (Electroless) Nickel-Phosphorus Coatings on
Metal1
This standard is issued under the fixed designation B733; 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* bondability, increased electrical conductivity, and resistance to

1.1 This specification covers requirements for autocatalytic strong alkali solutions.
(electroless) nickel-phosphorus coatings applied from aqueous 1.8 The medium phosphorous coatings (5 to 9 % P) are most
solutions to metallic products for engineering (functional) uses. widely used to meet the general purpose requirements of wear
1.2 The coatings are alloys of nickel and phosphorus pro- and corrosion resistance.
duced by autocatalytic chemical reduction with hypophosphite. 1.9 The high phosphorous (more than 10 % P) coatings
Because the deposited nickel alloy is a catalyst for the reaction, have superior salt-spray and acid resistance in a wide range of
the process is self-sustaining. The chemical and physical applications. They are used on beryllium and titanium parts for
properties of the deposit vary primarily with its phosphorus low stress properties. Coatings with phosphorus contents
content and subsequent heat treatment. The chemical makeup greater than 11.2 % P are not considered to be ferromagnetic.
of the plating solution and the use of the solution can affect the 1.10 Units—The values stated in SI units are to be regarded
porosity and corrosion resistance of the deposit. For more as standard.
details, see ASTM STP 265 (1)2 and Refs (2), (3), (4), and (5).
1.11 The following precautionary statement pertains only to
1.3 The coatings are generally deposited from acidic solu- the test method portion, Section 9, of this specification. This
tions operating at elevated temperatures. standard does not purport to address all of the safety concerns,
1.4 The process produces coatings of uniform thickness on if any, associated with its use. It is the responsibility of the user
irregularly shaped parts, provided the plating solution circu- of this standard to establish appropriate safety, health, and
lates freely over their surfaces. environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 The coatings have multifunctional properties, such as 1.12 This international standard was developed in accor-
hardness, heat hardenability, abrasion, wear and corrosion dance with internationally recognized principles on standard-
resistance, magnetics, electrical conductivity provide diffusion ization established in the Decision on Principles for the
barrier, and solderability. They are also used for the salvage of Development of International Standards, Guides and Recom-
worn or mismachined parts. mendations issued by the World Trade Organization Technical
1.6 The low phosphorus (2 to 4 % P) coatings are microc- Barriers to Trade (TBT) Committee.
rystalline and possess high as-plated hardness (620 to 750 HK
2. Referenced Documents
100). These coatings are used in applications requiring abra-
sion and wear resistance. 2.1 ASTM Standards:3
B368 Test Method for Copper-Accelerated Acetic Acid-Salt
1.7 Lower phosphorus deposits in the range between 1 %
Spray (Fog) Testing (CASS Test)
and 3 % phosphorus are also microcrystalline. These coatings
B374 Terminology Relating to Electroplating
are used in electronic applications providing solderability,
B380 Test Method for Corrosion Testing of Decorative
Electrodeposited Coatings by the Corrodkote Procedure
B487 Test Method for Measurement of Metal and Oxide
1
This specification is under the jurisdiction of ASTM Committee B08 on Coating Thickness by Microscopical Examination of
Metallic and Inorganic Coatings and is the direct responsibility of Subcommittee Cross Section
B08.03 on Engineering Coatings.
Current edition approved May 1, 2022. Published May 2022. Originally
3
approved in 1984. Last previous edition approved in 2021 as B733 – 21. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/B0733-22. contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
2
The boldface numbers given in parentheses refer to a list of references at the Standards volume information, refer to the standard’s Document Summary page on
end of the text. the ASTM website.

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 B733 − 22
B499 Test Method for Measurement of Coating Thicknesses Anodic Polarization Measurements
by the Magnetic Method: Nonmagnetic Coatings on G31 Guide for Laboratory Immersion Corrosion Testing of
Magnetic Basis Metals Metals
B504 Test Method for Measurement of Thickness of Metal- G59 Test Method for Conducting Potentiodynamic Polariza-
lic Coatings by the Coulometric Method tion Resistance Measurements
B537 Practice for Rating of Electroplated Panels Subjected G85 Practice for Modified Salt Spray (Fog) Testing
to Atmospheric Exposure 2.2 SAE Documents:5
B567 Test Method for Measurement of Coating Thickness AMS 2430 Shot Peening6
by the Beta Backscatter Method AMS 2590 Rotary Flap Peening of Metal Parts7
B568 Test Method for Measurement of Coating Thickness 2.3 ANSI Standard:8
by X-Ray Spectrometry ANSI/ASQ Z1.4 Sampling Procedures and Tables for In-
B571 Practice for Qualitative Adhesion Testing of Metallic spection by Attributes9
Coatings 2.4 Military Standard:10
B578 Test Method for Microindentation Hardness of Elec- MIL-STD-1916 DOD Preferred Methods of Acceptance of
troplated Coatings Product
B602 Guide for Attribute Sampling of Metallic and Inor- 2.5 ISO Standard:11
ganic Coatings ISO 4527 Metallic Coatings-Autocatalytic (Electroless)
B667 Practice for Construction and Use of a Probe for Nickel-Phosphorus Alloy Coatings—Specification and
Measuring Electrical Contact Resistance Test Methods
B678 Test Method for Solderability of Metallic-Coated
Products 3. Terminology
B697 Guide for Selection of Sampling Plans for Inspection 3.1 Definitions:
of Electrodeposited Metallic and Inorganic Coatings 3.1.1 significant surfaces, n—those substrate surfaces which
B762 Guide of Variables Sampling of Metallic and Inorganic the coating must protect from corrosion or wear, or both, and
Coatings that are essential to the performance.
B849 Specification for Pre-Treatments of Iron or Steel for
Reducing Risk of Hydrogen Embrittlement 3.2 Other Definitions—Terminology B374 defines most of
B850 Guide for Post-Coating Treatments of Steel for Reduc- the technical terms used in this specification.
ing the Risk of Hydrogen Embrittlement
4. Coating Classification
B851 Specification for Automated Controlled Shot Peening
of Metallic Articles Prior to Nickel, Autocatalytic Nickel, 4.1 The coating classification system provides for a scheme
or Chromium Plating, or as Final Finish to select an electroless nickel coating to meet specific perfor-
D1193 Specification for Reagent Water mance requirements based on alloy composition, thickness and
D2670 Test Method for Measuring Wear Properties of Fluid hardness.
Lubricants (Falex Pin and Vee Block Method) 4.1.1 TYPE describes the general composition of the de-
D2714 Test Method for Calibration and Operation of the posit with respect to the phosphorus content and is divided into
Falex Block-on-Ring Friction and Wear Testing Machine five categories which establish deposit properties (see Table 1).
D3951 Practice for Commercial Packaging NOTE 1—Due to the precision of some phosphorus analysis methods, a
D4060 Test Method for Abrasion Resistance of Organic deviation of 0.5 % has been designed into this classification scheme.
Coatings by the Taber Abraser Rounding of the test results due to the precision of the limits provides for
E60 Practice for Analysis of Metals, Ores, and Related an effective limit of 4.5 % and 9.5 %, respectively. For example, coating
Materials by Spectrophotometry with a test result for phosphorus of 9.7 % would have a classification of
TYPE V, see Appendix X5, Alloy TYPEs.
E140 Hardness Conversion Tables for Metals Relationship
Among Brinell Hardness, Vickers Hardness, Rockwell 4.2 Service Condition Based on Thickness:
Hardness, Superficial Hardness, Knoop Hardness, Sclero-
scope Hardness, and Leeb Hardness 5
Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale,
E156 Test Method for Determination of Phosphorus in PA 15096, http://www.sae.org.
6
High-Phosphorus Brazing Alloys (Photometric Method) The original reference MIL-S-13165 Shot Peening of Metal Parts was cancelled
(Withdrawn 1993)4 in February 1998 and referred to SAE AMS-S-13165, which was also cancelled and
superseded by AMS 2430.
E352 Test Methods for Chemical Analysis of Tool Steels and 7
The original reference MIL-R-81841 Rotary Flap Peening of Metal Parts was
Other Similar Medium- and High-Alloy Steels cancelled in April 2012 and referred to SAE AMS 2590.
8
F519 Test Method for Mechanical Hydrogen Embrittlement Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org.
Evaluation of Plating/Coating Processes and Service En- 9
The original reference MIL-STD-105 Sampling Procedures and Tables for
vironments Inspection by Attributes was cancelled in February 2008 and referred to MIL-
G5 Reference Test Method for Making Potentiodynamic STD-1916 or ANSI/ASQ Z1.4.
10
Available from Standardization Documents Order Desk, Bldg. 4 Section D,
700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
11
Available from International Organization for Standardization (ISO), ISO
4
The last approved version of this historical standard is referenced on Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
www.astm.org. Switzerland, https://www.iso.org.

2
 B733 − 22
TABLE 1 Deposit Alloy Types TABLE 3 Classification of Post Heat Treatment
Type Phosphorus % wt Temperature
Class Description Time (h)
I No Requirement for Phosphorus (°C)
II 1 to 3 1 No Heat Treatment, As Plated
III 2 to 4 2 Heat Treatment for Maximum Hardness
IV 5 to 9 TYPE I 260 20
V 10 and above 285 16
320 8
400 1
TYPE II 350 to 380 1
TYPE III 360 to 390 1
TYPE IV 365 to 400 1
4.2.1 Service condition numbers are based on the severity of TYPE V 375 to 400 1
the exposure in which the coating is intended to perform and 3 Adhesion on Steel 180 to 200 2 to 4
4 Adhesion, Carburized Steel and 120 to 130 1 to 6
minimum coating thickness to provide satisfactory perfor- Age Hardened Aluminum
mance (see Table 2). 5 Adhesion on Beryllium and 140 to 150 1 to 2
4.2.2 SC0 Minimum Service, 0.1 µm—This is defined by a Aluminum
6 Adhesion on Titanium 300 to 320 1 to 4
minimum coating thickness to provide specific material prop-
erties and extend the life of a part or its function. Applications
include requirements for diffusion barrier, undercoat, electrical
conductivity, and wear and corrosion protection in specialized
environments.
4.2.3 SC1 Light Service, 5 µm—This is defined by a 4.3.3 Class 3—Heat treatment at 180 °C to 200 °C for 2 h to
minimum coating thickness of 5 µm for extending the life of 4 h to improve coating adhesion on steel and to provide for
the part. Typical environments include light-load lubricated hydrogen embrittlement relief (see 6.6).
wear, indoor corrosion protection to prevent rusting, and for 4.3.4 Class 4—Heat treatment at 120 °C to 130 °C for 1 h to
soldering and mild abrasive wear. 6 h to increase adhesion of carburized steel or heat-treatable
4.2.4 SC2 Mild Service, 13 µm—This is defined by mild (age-hardened) aluminum alloys (see Note 3).
corrosion and wear environments. It is characterized by indus- 4.3.5 Class 5—Heat treatment at 140 °C to 150 °C for 1 h to
trial atmosphere exposure on steel substrates in dry or oiled 2 h to improve coating adhesion for aluminum, non age-
environments. hardened aluminum alloys, copper, copper alloys, or beryllium.
4.2.5 SC3 Moderate Service, 25 µm—This is defined by 4.3.6 Class 6—Heat treatment at 300 °C to 320 °C for 1 h to
moderate environments such as non marine outdoor exposure, 4 h to improve coating adhesion for titanium alloys.
alkali salts at elevated temperature, and moderate wear. NOTE 3—Heat-treatable aluminum alloys such as Type 7075 can
4.2.6 SC4 Severe Service, 75 µm—This is defined by a very undergo microstructural changes and lose strength when heated to over
aggressive environment. Typical environments would include 130 °C.
acid solutions, elevated temperature and pressure, hydrogen
sulfide and carbon dioxide oil service, high-temperature chlo- 5. Ordering Information
ride systems, very severe wear, and marine immersion. 5.1 The following information shall be supplied by the
NOTE 2—The performance of the autocatalytic nickel coating depends purchaser in either the purchase order or on the engineering
to a large extent on the surface finish of the article to be plated and how drawing of the part to be plated:
it was pretreated. Rough, non uniform surfaces require thicker coatings 5.1.1 Title, ASTM designation number, and year of issue of
than smooth surfaces to achieve maximum corrosion resistance and this specification.
minimum porosity.
5.1.2 Classification of the coating by type, service
4.3 Post Heat Treatment Class—The nickel-phosphorus condition, class (see 4.1, 4.2, and 4.3).
coatings shall be classified by heat treatment after plating to 5.1.3 Specify maximum dimension and tolerance
increase coating adhesion or hardness, or both (see Table 3). requirements, if any.
4.3.1 Class 1—As-deposited, no heat treatment. 5.1.4 Peening, if required (see 6.3).
4.3.2 Class 2—Heat treatment at 260 °C to 400 °C to 5.1.5 The tensile strength of the material in MPa (see 6.3.1
produce a minimum hardness of 850 HK100. and 6.6).
5.1.6 Stress relief heat treatment before plating (see 6.3).
5.1.7 Hydrogen Embrittlement Relief after plating (see 6.6).
TABLE 2 Service Conditions 5.1.8 Significant surfaces and surfaces not to be plated must
Coating Thickness Requirements be indicated on drawings or sample.
Minimum Coating 5.1.9 Supplemental or Special Government Requirements
Service Condition Thickness µm in.
Specification such as, specific phosphorus content, abrasion wear or corro-
SC0 Minimum Thickness 0.1 0.000004 sion resistance of the coating, solderability, contact resistance
SC1 Light Service 5 0.0002 and packaging selected from Supplemental Requirements.
SC2 Mild Service 13 0.0005 5.1.10 Requirement for a vacuum, inert, or reducing atmo-
SC3 Moderate Service 25 0.001
SC4 Severe Service 75 0.003 sphere for heat treatment above 260 °C to prevent surface
oxidation of the coating (see S1.3).

3
 B733 − 22
5.1.11 Test methods for coating adhesion, composition, 6.5 Plating Process:
thickness, porosity, wear and corrosion resistance, if required, 6.5.1 To obtain consistent coating properties, the bath must
selected from those found in Section 9 and Supplemental be monitored periodically for pH, temperature, nickel, and
Requirements. hypophosphite. Replenishments to the plating solution should
5.1.12 Requirements for sampling (see Section 8). be as frequent as required to maintain the concentration of the
NOTE 4—The purchaser should furnish separate test specimens or nickel and hypophosphite between 90 % and 100 % of set
coupons of the basis metal for test purposes to be plated concurrently with point. The use of a statistical regimen to establish the control
the articles to be plated (see 8.4). limits and frequency of analysis may be employed to ensure
quality deposits are produced.
6. Materials and Manufacture 6.5.2 Mechanical movement of parts, agitation of the bath,
6.1 Substrate—Defects in the surface of the basis metal such and filtration is recommended to increase coating smoothness
as scratches, porosity, pits, inclusions, roll and die marks, laps, and uniformity and prevent pitting or streaking due to hydro-
cracks, burrs, cold shuts, and roughness may adversely affect gen bubbles.
the appearance and performance of the deposit, despite the 6.6 Post Coating Treatment for Iron and Steel for Reducing
observance of the best plating practice. Any such defects on the Risk of Hydrogen Embrittlement—Parts that are made of
significant surfaces shall be brought to the attention of the steel with ultimate tensile strengths of 1000 MPa (correspond-
purchaser before plating. The producer shall not be responsible ing hardness values 300 HV10, 303 HB, or 31 HRC or greater),
for coatings defects resulting from surface conditions of the as well as surface hardened parts, shall require post coating
metal, if these conditions have been brought to the attention of hydrogen embrittlement relief baking when specified by the
the purchaser. purchaser. The tensile strength shall be supplied by the
6.2 Pretreatment—A suitable method shall activate the sur- purchaser. Guide B850 contains a list of post treatments,
face and remove oxide and foreign materials, which may cause procedures, limitations, and guidelines that are permitted to be
poor adhesion and coating porosity. used to reduce the effects of hydrogen embrittlement.
6.6.1 Heat treatment shall be performed preferably within
NOTE 5—Heat treatment of the base material may affect its metallur-
gical properties. An example is leaded steel which may exhibit liquid or 1 h, but not more than 3 h, of plating unless the size or weight
solid embrittlement after heat treatment. Careful selection of the pre and of the part prevents the initiation of heart treatment within 3 h.
post heat treatments are recommended. In this case, the part shall be heat treated as soon as possible.
6.3 Stress Relief: In all cases, the duration of the heat treatment shall commence
6.3.1 Pretreatment of Iron and Steel for Reducing the Risk of from the time at which the whole of each part attains the
Hydrogen Embrittlement—Parts that are made of steel with specified temperature.
ultimate tensile strength of greater than 1000 MPa (hardness of 6.7 Heat Treatment After Plating to Improve Adhesion—To
31 HRC), that have been machined, ground, cold formed, or improve the adhesion of the coating to various substrates, the
cold straightened subsequent to heat treatment require stress heat treatments in Table 3 should be performed as soon as
relief heat treatment when specified by the purchaser. The practical after plating (see 4.3).
tensile strength of the material shall be supplied by the
purchaser. Specification B849 contains a list of pre-treatments, 6.8 Heat Treatment After Plating to Increase Hardness:
precautions, procedures, and caveats that shall be used. 6.8.1 To increase the hardness of the coating, a heat treat-
6.3.2 Peening—Peening prior to plating may be required on ment of over 260 °C is required. Table 3 describes the heat
high-strength steel parts to induce residual compressive treatment for maximum hardness. See Appendix X3 and
stresses in the surface, which can reduce loss of fatigue Appendix X4.
strength and improve stress corrosion resistance after plating. 6.8.2 A heat treatment at 260 °C for greater than 20 h should
(See Supplementary Requirements.) be used to reduce the loss of surface hardness and strength of
6.3.2.1 Steel parts which are designed for unlimited life some ferrous basis metals. Avoid rapid heating and cooling of
under dynamic loads shall be shot peened or rotary flap peened. plated parts. Sufficient time must be allowed for large parts to
reach oven temperature.
NOTE 6—Controlled shot peening is the preferred method because there
are geometry’s where rotary flap peening is not effective. See S1.11.2. 6.8.3 Do not use gas containing hydrogen with high-
strength steel parts.
6.3.2.2 Unless otherwise specified, the shot peening shall be
accomplished on all surfaces for which the coating is required NOTE 7—The length of time to reach maximum hardness varies with the
and all immediate adjacent surfaces when they contain notches, phosphorus content of the deposit. High phosphorus deposits may require
longer time or a higher temperature, or both. Individual alloys should be
fillets, or other abrupt changes of section size where stresses tested for maximum hardness attainable, especially for conditions of lower
will be concentrated. temperatures and longer times.
6.4 Racking—Parts should be positioned so as to minimize NOTE 8—Inert or reducing atmosphere or vacuum sufficient to prevent
oxidation is recommended for heat treatment above 260 °C.
trapping of hydrogen gas in cavities and holes, allowing free
circulation of solution over all surfaces to obtain uniform
7. Requirements
coating thickness. The location of rack or wire marks in the
coating shall be agreed upon between the producer and 7.1 Process—The coating shall be produced from an aque-
purchaser. ous solution through chemical reduction reaction.

4
 B733 − 22
7.2 Acceptance Requirements—These requirements are otherwise specified by purchaser in the purchase order or
placed on each lot or batch and can be evaluated by testing the contract (see 5.1.12 and S1.11.1). Guide B697 and Test Method
plated part. B762 also contain sampling plans that are designed for the
7.2.1 Appearance: sampling inspection of coatings. When Guide B697 or Test
7.2.1.1 The coating surface shall have a uniform, metallic Method B762 are specified, the purchaser and producer must
appearance without visible defects such as blisters, pits, agree on the plan to be used.
pimples, and cracks.
NOTE 10—Usually, when a collection of coated parts (the inspection lot
7.2.1.2 Imperfections that arise from surface conditions of 8.2) is examined for compliance with the requirements placed on the parts,
the substrate which the producer is unable to remove using a relatively small number of parts, the sample, is selected at random and
conventional pretreatment techniques and that persist in the inspected. The inspection lot is then classified as complying or not
coating shall not be cause for rejection (see 6.1). Also, complying with the requirements based on the results of the inspection
sample. The size of the sample and the criteria of compliance are
discoloration due to heat treatment shall not be cause for determined by the application of statistics. The procedure is known as
rejection unless special heat treatment atmosphere is specified sampling inspection.
(see 5.1.10). Test Method B602 contains four sampling plans, three for use with tests
7.2.2 Thickness—The thickness of the coating shall exceed that are nondestructive and one for use with tests that are destructive. The
the minimum requirements in Table 2 as specified by the purchaser and producer may agree on the plan(s) to be used. If they do not,
Test Method B602 identifies the plan to be used.
service condition agreed to prior to plating. After coating and Guide B697 provides a large number of plans and also gives guidance
if specified, the part shall not exceed maximum dimension on on the selection of a plan.
significant surface (see 5.1.3). Test Method B762 can be used only for coating requirements that have
a numerical limit, such as coating thickness. Test Method B762 contains
NOTE 9—The thickness of the coating cannot be controlled in blind or several plans and also gives instructions for calculating plans to meet
small diameter deep holes or where solution circulation is restricted. special needs. The purchaser and producer may agree on the plan(s) to be
7.2.3 Adhesion—The coating shall have sufficient adhesion used. If they do not, Test Method B762 identifies the plan to be used.
An inspection lot shall be defined as a collection of coated parts which
to the basis metal to pass the specified adhesion test (see 9.4 are of the same kind, that have been produced to the same specification,
and Practice B571). that have been coated by a single producer at one time or approximately
7.2.4 Porosity—The coatings shall be essentially pore free the same time under essentially identical conditions, and that are submit-
when tested according to one of the methods of 9.6. The test ted for acceptance or rejection as a group.
method, the duration of the test, and number of allowable spots 8.3 All specimens used in the sampling plan for acceptance
per unit area shall be specified (see 5.1.11). tests shall be made of the same basis material and in the same
7.3 Qualification Requirements—These requirements are metallurgical condition as articles being plated to this specifi-
placed on the deposit and process and are performed on cation.
specimens to qualify the deposit and plating process. The tests 8.4 All specimens shall be provided by the purchaser unless
for these qualification requirements shall be performed otherwise agreed to by the producer.
monthly or more frequently.
7.3.1 Composition—Type II, III, IV, V deposits shall be NOTE 11—The autocatalytic nickel process is dynamic and a daily
analyzed for alloy composition by testing for phosphorus (see sampling is recommended. For coatings requiring alloy analysis and
corrosion testing, weekly sampling should be considered as an option.
9.1). The weight percent of phosphorus shall be in the range
designated by type classification (see 4.1). 9. Test Methods
7.3.2 Microhardness—The microhardness of Class 2 depos-
its shall be determined by Test Method B578 (Knoop). For 9.1 Deposit Analysis for Phosphorus:
Class 2 coatings, the microhardness shall equal or exceed a 9.1.1 Phosphorus Determination—Determine mass % phos-
minimum of 850 HK100 (or equivalent Vickers) (see 4.3 and phorus content according to Practice E60, Test Methods E352,
9.5). The conversion of Vickers to Knoop using Tables E140 is or Test Method E156 on known weight of deposit dissolved in
not recommended. warm concentrated nitric acid.
7.3.3 Hydrogen Embrittlement—The process used to deposit 9.1.2 Composition can be determined by atomic absorption,
a coating onto high strength steels shall be evaluated for emission, or X-ray fluorescence spectrometry.
hydrogen embrittlement by Test Method F519.
NOTE 12—Inductively coupled plasma techniques can determine the
alloy to within 0.1 %. The following analysis wavelength lines have been
8. Sampling used with minimum interference to determine the alloy.
8.1 The purchaser and producer are urged to employ statis- Ni 216.10 nm Cd 214.44 nm Fe 238.20 nm
P 215.40 nm Co 238.34 nm Pb 283.30 nm
tical process control in the coating process. Properly performed P 213.62 nm Cr 284.32 nm Sn 198.94 nm
this will ensure coated products of satisfactory quality and will Al 202.55 nm Cu 324.75 nm Zn 206.20 nm
reduce the amount of acceptance inspection. 9.2 Appearance—Examine the coating visually for compli-
8.1.1 Sampling plans can only screen out unsatisfactory ance with the requirements of 7.2.1.
products without assurance that none of them will be accepted
(6). 9.3 Thickness—Measure the coating thickness for compli-
ance with the requirements of 7.2.2.
8.2 The sampling plan used for the inspection of a quantity
of coated parts (lot) shall be Test Method B602 unless NOTE 13—Eddy-current type instruments give erratic measurements

5
 B733 − 22
due to variations in conductivity of the coatings with changes in the coating on the tension side of the bend are not an indication
phosphorus content. of poor adhesion. Insertion of a sharp probe at the interface of
9.3.1 Microscopical Method—Measure the coating thick- the coating and basis metal to determine the adhesion is
ness of a cross section according to Test Method B487. suggested.
NOTE 14—To protect the edges, electroplate the specimens with a NOTE 17—Appropriate test specimens are strips approximately 25 mm
minimum of 5 µm of nickel or copper prior to cross sectioning. to 50 mm wide, 200 mm to 300 mm long, and 3 mm to 6 mm thick.
9.3.2 Magnetic Induction Instrument Method—Test Method 9.4.2 Impact Test—A spring-loaded center punch with a
B499 is applicable to magnetic substrates plated with autocata- point having 2 mm to 3 mm radius is used to test adhesion of
lytic nickel deposits that contain more than 11 mass % the coating on nonsignificant surfaces of the plated part. Make
phosphorus (not ferromagnetic) and that have not been heat- three closely spaced indentations and examine under 10×
treated. The instrument shall be calibrated with deposits plated magnification for flaking or blistering of the coating, which is
in the same solution under the same conditions on magnetic cause for rejection.
steel. 9.4.3 Thermal Shock—The coated part is heated to 200 °C
9.3.3 Beta Backscatter Method—Test Method B567 is only in an oven and then quenched in room temperature water. The
applicable to coatings on aluminum, beryllium, magnesium, coating is examined for blistering or other evidence of poor
and titanium. The instrument must be calibrated with standards adhesion at 4× magnification.
having the same composition as the coating. 9.5 Microhardness—The microhardness of the coating can
NOTE 15—The density of the coating varies with its mass % phosphorus be measured by Test Method B578 using Knoop indenter and
content (See Appendix X2). is reported in Knoop Hardness Number (HK). It will vary
depending on loads, type of indenter, and operator. A 100 g
9.3.4 Micrometer Method—Measure the part, test coupon,
load is recommended. The rhombic Knoop indenter gives
or pin in a specific spot before and after plating using a suitable
higher hardness readings than the square-base pyramidal Vick-
micrometer. Make sure that the surfaces measured are smooth,
ers diamond indenter for 100 g to 300 g loads; see Ref (7). For
clean, and dry.
maximum accuracy, a minimum coating thickness of 75 µm is
9.3.5 Weigh, Plate, Weigh Method—Using a similar sub-
recommended. Conversions of Vickers or Knoop hardness
strate material of known surface area, weigh to the nearest
number to Rockwell C is not recommended.
milligram before and after plating, making sure that the part or
coupon is dry and at room temperature for each measurement. NOTE 18—On thick (75 µm+) coatings on steel a surface microhardness
Calculate the thickness from the increase in mass, specific determination is permissible.
gravity, and area as follows: 9.6 Porosity—There is no universally accepted test for
coating thickness, µm 5 10 W/ ~ A 3 D ! (1) porosity. When required, one of the following tests can be used
on the plated part or specimen.
where: 9.6.1 Ferroxyl Test for Iron Base Substrates—Prepare the
W = mass gain, mg, test solution by dissolving 25 g of potassium ferricyanide and
A = total surface area, cm2, and 15 g of sodium chloride in 1 L of distilled water. After
D = specific gravity, g/cm3 (see Appendix X2). cleaning, immerse the part for 30 s in the test solution at 25 °C.
9.3.6 Coulometric Method—Measure the coating thickness After rinsing and air drying, examine the part for blue spots,
in accordance with Test Method B504. The solution to be used which form at pore sites.
shall be in accordance with manufacturer’s recommendations. 9.6.2 Boiling Water Test for Iron-Base Substrates—
The surface of the coating shall be cleaned prior to testing (see Completely immerse the part to be treated in a vessel filled
Note 14). with aerated water at room temperature. Apply heat to the
9.3.6.1 Calibrate standard thickness specimens with depos- beaker at such a rate that the water begins to boil in not less
its plated in the same solution under the same conditions. than 15 min, nor more than 20 min after the initial application
9.3.7 X-Ray Spectrometry—Measure the coating thickness of heat. Continue to boil the water for 30 min. Then remove the
in accordance with Test Method B568. The instrument must be part, air dry, and examine for rust spots, which indicate pores.
calibrated with standards having the same composition as the NOTE 19—Aerated water is prepared by bubbling clean compressed air
coating. through distilled water by means of a glass diffusion disk at room
temperature for 12 h. The pH of the aerated water should be 6.7 + 0.5 pH.
NOTE 16—This method is only recommended for deposits in the
as-plated condition. The phosphorus content of the coating must be known 9.6.3 Aerated Water Test for Iron-Base Substrates—
to calculate the thickness of the deposit. Matrix effect due to the Immerse the part for 4 h in vigorously aerated Type IV or better
distribution of phosphorus in layers of the coating also effect the water (see Specification D1193) at 25 °C 6 2 °C temperature
measurement accuracy and require that calibration standards be made and then examine the part for rust spots.
under the same conditions as the production process.
9.6.4 Alizarin Test for Aluminum Alloys—Wipe the plated
9.4 Adhesion: part or specimen with 10 mass % sodium hydroxide solution.
9.4.1 Bend Test (Practice B571)—A sample specimen is After 3 min contact, rinse, and apply a solution of alizarin
bent 180° over a mandrel diameter 4× the thickness (10 mm sulfonate prepared by dissolving 1.5 g of methyl cellulose in
minimum) of the specimen and examined at 4× power magni- 90 mL of boiling water to which, after cooling, 0.1 g sodium
fication for flaking or separation at the interface. Fine cracks in alizarin sulfonate, dissolved in 5 mL of ethanol is added. After

6
 B733 − 22
4 min contact, apply glacial acetic acid until the violet color producer promptly in writing. In the case of dissatisfaction
disappears. Any red spots remaining indicate pores. with the results of a test, the producer may make a claim for a
9.6.5 Porosity Test for Copper Substrates—Wipe the plated rehearing. Coatings that show imperfections may be rejected.
part or specimen with glacial acetic acid. After 3 min, apply a
solution of potassium ferrocyanide prepared by dissolving 1 g 11. Certification
of potassium ferrocyanide and 1.5 g methyl cellulose in 90 mL
of boiling distilled water. The appearance of brown spots after 11.1 When specified in the purchase order or contract, the
2 min indicate pores. purchaser shall be furnished certification that the samples
representing each lot have been processed, tested and inspected
9.7 Other Test Methods—Test methods which have been as directed in this specification and the requirements have been
developed that are equal to or better than these may be met. When specified in the purchase order or contract, a report
substituted. The precision and bias requirements will vary for of the test results shall be furnished.
each type of test. If an alternate test is specified it shall be
agreed upon between the producer and the purchaser. 12. Keywords
10. Rejection and Rehearing 12.1 autocatalytic; chemical nickel; coatings; conductive;
10.1 Part(s) that fail to conform to the requirements of this corrosion resistance; electroless; functional; nickel; nickel
specification may be rejected. Rejection shall be reported to the phosphorus; wear resistance

SUPPLEMENTARY REQUIREMENTS

The following supplementary requirements shall apply only when specified by the purchaser in the
contract or order.

S1.1 Shot Peening—When specified by the purchaser in the S1.7 Contact Resistance—When specified by the purchaser
ordering information, the part(s) shall be shot peened prior to in the ordering information, the coating shall be tested for
plating in accordance with Specification B851 or AMS 2430. contact resistance using Practice B667.
S1.2 Composition—When specified by the purchaser in the S1.8 Solderability—When specified by the purchaser in the
ordering information, the phosphorus content shall be main- ordering information, the unaged coating shall pass Test
tained in the deposit to within 1 %. Use the test methods Method B678 on solderability.
described in 9.1. S1.9 Corrosion Resistance—When specified by the pur-
S1.3 Inert Atmosphere—When specified by the purchaser in chaser in the ordering information, the coating shall pass any
the ordering information, the coating shall be heat treated in a special corrosion tests agreed to by the producer. The corrosion
vacuum, or an inert or reducing atmosphere to prevent surface resistance of the coating to a specific liquid medium can be
oxidation of the coating. determined by means of immersion tests (see Practice G31) or
electrochemical test (see Test Method G5 or Practice G59).
S1.4 Hydrogen Embrittlement—When specified by the pur- S1.10 Pitting Corrosion Resistance—Use Practice G85
chaser in the ordering information, the plating process shall be (acetic acid-salt spray test), Test Method B368 (copper-
evaluated at the time of processing parts for hydrogen em- accelerated acetic acid-salt spray, CASS), or Test Method B380
brittlement using Test Method F519. (Corrodkote) to evaluate the corrosion resistance of the coating
S1.5 Abrasive Wear—When specified by the purchaser in to pitting.
the ordering information, the coating shall be tested for S1.11 Special Government Requirements:
abrasion wear resistance using the method in Appendix X1 of S1.11.1 Sampling—Part(s) plated for the US Government or
this specification. The coating shall meet a maximum wear rate Military use shall use MIL-STD-1916 or ANSI/ASQ Z1.4 as
which is specified by the purchaser and agreed to by the the sampling plan.
producer. S1.11.2 Shot Peening—High strength steel part(s) pro-
S1.6 Adhesive Wear—When specified by the purchaser in cessed for US Government or Military use shall be shot peened
the ordering information, the coating shall be tested for in accordance with AMS 2430 or rotary flap peened in
adhesive wear resistance using Test Method D2714 or Test accordance with AMS 2590 (see Note 6).
Method D2670. The wear rate shall be specified by the S1.11.3 Packaging—Parts shall be packaged in accordance
purchaser and agreed to by the producer. with Practice D3951.

7
 B733 − 22
APPENDIXES

(Nonmandatory Information)

X1. TABER ABRASER WEAR TEST METHOD

X1.1 Scope X1.2.5 Analytical Balance—Capable of weighing 150 g 6

X1.1.1 This test method will evaluate the resistance of the 0.1 mg.
coating to abrasive wear. The test is performed by rotating a X1.3 Conditioning
plated panel under weighted abrasive wheels. Abrasion resis-
tance is calculated as loss in weight by weighing the panel after X1.3.1 Condition the plated panel under settings of humid-
each 1000 cycles. Duration of the test is 6000 cycles and it can ity and temperature as agreed upon between the interested
be extended to 25 000 cycles for more complete results. parties. If no settings are specified, condition the coated panel
for at least 24 h at 23 °C 6 2 °C and 50 % 6 5 % relative
NOTE X1.1—Variation in results have been attributed to calibration of humidity. Conduct the test in the same environment or imme-
the instrument, the humidity in the laboratory, and the storage conditions
of the CS-10 wheels. diately on removal therefrom.
X1.1.2 The results may be variable between tests and X1.4 Procedure
therefore three plated test specimens should be tested to 6000
X1.4.1 Plate three specimens with 0.001 in. (25 µm) of
cycles each. The results should be averaged without the first
nickel phosphorus coating.
1000 cycles and the abrasion wear resistance is reported as the
weight loss in mg/1000 cycles (Taber Wear Index). X1.4.2 Prepare the Taber Abraser such that a load of 1000 g
(per wheel) is used. Adjust the vacuum nozzle gap to 3 mm 6
X1.1.3 This international standard was developed in accor-
1 mm above the specimen surface. Set the vacuum suction
dance with internationally recognized principles on standard-
force to 100.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- X1.4.3 Subject each of the three specimens to abrasion
mendations issued by the World Trade Organization Technical using the following steps:
Barriers to Trade (TBT) Committee. X1.4.3.1 Reface the CS-10 wheels with a S-11 refacing disc
for 50 cycles, then run CS-10 wheels on the coating for 1000
X1.2 Apparatus cycles to remove any surface roughness.
X1.4.3.2 Brush the specimen to remove any debris, then
X1.2.1 Taber Abraser Wear Testing Unit—As described in
weigh the specimen to the nearest 0.1 mg.
Test Method D4060, the unit must be capable of loading each
X1.4.3.3 Resurface the CS-10 wheels with a new S-11
wheel with 1000 g load and operating with a vacuum.
refacing disc for 50 cycles.
X1.2.2 Abrasion Wheels12—Use CS-10 (resilient rubber) X1.4.3.4 Abrasion test the coating with 1000 g load per
Taber wheels. The wheels shall be cylindrically shaped, have a wheel for 1000 cycles.
diameter between 52.4 mm and 44.4 mm, a width of 12.7 mm X1.4.3.5 Repeat X1.4.3.2, X1.4.3.3, and X1.4.3.4 until a
6 0.3 mm, and an axial hole 16.0 mm 6 0.1 mm to allow the total of 6000 cycles, or more if desired, have been accom-
wheel to be mounted to the wear testing unit. The hardness of plished for each specimen. After final abrasion, weigh the
CS-10 wheels can change with time and can affect the specimen to the nearest 0.1 mg.
reproducibility of results (see Test Method D4060). Wheels
NOTE X1.2—Weight loss measurements are recorded after every 1000
should not be used after the date marked on them.
cycles, but only the weight of the test specimen after the 1000 cycle
X1.2.3 Refacing Medium—Taber S-11 abrasive disc, used break-in period and weight of the test specimen after final abrasion are
for resurfacing the CS-10 wheels. The refacing medium shall used to determine Wear Index and Weight Loss. The weight loss
measurements may be used to plot rate of abrasion if desired.
be silicon carbide coated abrasive with an average particle size
of 92 µm (150 grit CAMI-grade), approximately 100 mm X1.5 Calculation
diameter with a 7 mm center hole.
X1.5.1 Wear Index—Compute the wear index, I, of a test
X1.2.4 Test Specimens—Test specimens shall be made from specimen as follows:
20 gauge CR steel 4 in. by 4 in. (100 mm by 100 mm by
1.3 mm) with a 0.250 in. (6.35 mm) hole in the center. Test ~ A 2 B ! 1000
I5 (X1.1)
C
panels must have both surfaces substantially plane and parallel,
and are available from Taber. where:
A = weight of test specimen after 1000 cycle break-in
period, mg,
12
The sole source of supply known to the committee at this time is Taber B = weight of test specimen after final abrasion, mg, and
Industries, North Tonawanda, NY. If you are aware of alternative suppliers, please C = number of cycles of abrasion recorded.
provide this information to ASTM International Headquarters. Your comments will
receive careful consideration at a meeting of the responsible technical committee, X1.5.2 Weight Loss—Compute weight loss, L, of the test
which you may attend. specimen as follows:

8
 B733 − 22
L5A2B (X1.2) X1.6 Reporting
where: X1.6.1 Determine the average weight loss in milligrams for
A = weight of test specimen after 1000 cycle break-in each specimen per 1000 cycles (Taber Wear Index) and the
period, mg, and mean weight loss in milligrams for all specimens. Report the
B = weight of test specimen after final abrasion, mg. mean and standard deviation for the coating.

9
 B733 − 22

X2. DENSITY OF AUTOCATALYTIC NICKEL DEPOSITS

FIG. X2.1 Density of Autocatalytic Nickel Phosphorus Alloy Summary of Reported Values

10
 B733 − 22

X3. HARDNESS VERSUS 1 H HEAT TREATMENT

FIG. X3.1 Hardness of Autocatalytic Nickel Phosphorus Versus 1 h Heat Treatment Versus Phosphorus

X3.1 This graph presents information on the relationship of X3.2 The ultimate hardness of the deposit is dependent on
hardness and heat treatment for 1 h for different phases which the time and temperature of heat treatment as well as the
approximate the TYPEs. Deposits that are low in phosphorus phosphorus content, age of the solution, concentration of
(β) are harder as plated and will transition between 200 °C and hypophosphite, and type of additive system used. Type I and
400 °C, producing a mixture of fcc Ni and Ni3P. Deposits that IV deposits are subject to greater structural variation and their
are high in phosphorus (γ) are softer in the as plated condition properties are less predictable.
and will also transition between 275 °C and 350 °C, producing
a mixture of fcc Ni and Ni3P. Deposits in the range of 4 % to X3.3 Fig. X3.1 and Appendix X4 can be used to approxi-
8 % are a mixture of both β and γ and have properties that are mate the hardness after heat treatment.
less predictable after heat treatment.

11
 B733 − 22

X4. HARDNESS VERSUS TIME AND TEMPERATURE

NOTE 1—These graphs are average and may vary with deviations from normal practice.
FIG. X4.1 Hardness and Annealing Time Versus Temperature
9 % Phosphorus Deposit

X4.1 Fig. X4.1 provides information on the effect of anneal- tation hardening at 200 °C. Deposits higher than 7.5 % will be
ing time on the precipitation of nickel and 9 % phosphorus to stronger and when the deposit reaches around 11.2 % will be
Ni3P and fcc Ni. Alloys of other phosphorus contents have saturated with phosphorus. The precipitation of these high
differing hardness versus time and temperature. Deposits that phosphorus deposits may be delayed for several minutes in the
are less than 7.5 % will have lower strength and start precipi- mid-range temperatures.

12
 B733 − 22

X5. ALLOY TYPES

FIG. X5.1 Selected Properties of As Plated Autocatalytic Nickel Phosphorus Coatings by Phosphorus Content

NOTE X5.1—These different alloy TYPEs are produced from processes point. These differences are produced by micro structural
which are specifically formulated and controlled. Additional requirements differences between Ni + Ni3P and Ni3P. These differences
for internal stress, purity, and elongation may be necessary for some
applications. also effect non-destructive thickness testing by X-Ray and
magnetic means. Careful attention to the selection of TYPE
X5.1 The physical differences of these TYPEs provide for a will insure optimum performance of the deposit in the intended
wide variation in performance in wire bonding, contact application.
resistance, machineability, lubricity, reactivation, and melting

13
 B733 − 22

X6. SUMMARY PROGRAM 14

TABLE X6.1 Results of 110 Month Exposure of Autocatalytic (Electroless) Nickel Deposits at Kure Beach, North CarolinaA
Phosphorus Alloy % wt Practice
Heat Thickness, Thickness,
Deposit Type Source Lot Surface B537 Ratings
Treatment µm Target µm Actual ICP EDAX 110 Months
1 Smooth No 12.5 3.6 ± 3.0
2 Smooth No 25 9.2 ± 0.3
V G 3 Smooth No 75 80.5 10.5 10.9 10 ± 0
4 Smooth Yes 25 9.2 ± 0.3
5 Ground No 25 7.8 ± 0.4
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 8.0 ± 0
V E 3 Smooth No 75 77 10.0 10.2 9.8 ± 0.4
4 Smooth Yes 25 8.2 ± 0.8
5 Ground No 25 4.2 ± 0.4
1 Smooth No 12.5 6.8 ± 1.3
2 Smooth No 25 6.2 ± 0.4
V C 3 Smooth No 75 46 9.9 10.4 8.8 ± 1.1
4 Smooth Yes 25 6.8 ± 1.3
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 5.8 ± 0.4
IV J 3 Smooth No 75 9.0 9.6 ± 1.1
4 Smooth Yes 25 7.0 ± 0
5 Ground No 25 1.0 ± 2
1 Smooth No 12.5 0.6 ± 0.5
2 Smooth No 25 7.4 ± 0.9
IV H 3 Smooth No 75 8.9 10.0 ± 0
4 Smooth Yes 25 4.8 ± 1.1
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 1.8 ± 1.6
IV B 3 Smooth No 75 79 8.3 7.3 6.0 ± 1.0
4 Smooth Yes 25 5.0 ± 0
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 0.0 ± 0
IV D 3 Smooth No 75 77 8.2 9.5 5.0 ± 1.4
4 Smooth Yes 25 5.4 ± 0.5
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 0.0 ± 0
IV K 3 Smooth No 75 7.5 0.6 ± 0.8
4 Smooth Yes 25 5.6 ± 2.8
5 Ground No 25 0.0 ± 0
1 Smooth No 12.5 0.0 ± 0
2 Smooth No 25 0.2 ± 0.4
IV I 3 Smooth No 75 80 7.1 0.4 ± 0.5
4 Smooth Yes 25 4.6 ± 0.8
5 Ground No 25 0.0 ± 0
A
The conclusions from this marine exposure program have been summarized by Dr. George DiBari of INCO in his paper Marine Corrosion Performance of EN Coating
on Steel, Final Report on ASTM Program 14 which was presented at EN91 Conference, Product Finishing.

X6.1 Results of 110 Month Exposure of Autocatalytic higher than typical processing and was chosen to evaluate the
Nickel Deposits at Kure Beach, North Carolina: formation of diffusion products of iron, nickel and phosphorus.
X6.1.1 Program 14 is part of an ongoing marine exposure X6.1.3 The following matrix of test panels were prepared
testing process at the 75 m site at LaQue Center for Corrosion and exposed with subsequent analysis for alloy and thickness.
Technology, Wrightsville, NC (Kure Beach). The program Panels were rated at Kure Beach each year by a team from
called for the plating of both Type IV and Type V deposits on ASTM Committee B08 using Practice B537.
standard smooth and ground steel Q Panels. X6.1.4 The interpretation of the results of these exposure
X6.1.2 There were nine different sources of deposits, each test should be made on the basis of general performance of the
providing five lots of five panels. The program involved plating coating on panels. Base metal condition, undercoats, surface
12.5 µm, 25 µm, and 75 µm thicknesses on smooth and ground preparation, and post processing all have a significant effect on
surface and one smooth lot heat treated for hardness at 550 °C the performance and should be given careful consideration
for 2 h. The heat treatment temperature was considerably when designing the part and pretreatment processing sequence.

14
 B733 − 22

X7. STRIPPING AND REWORK

X7.1 The stripping of electroless nickel deposits requires These solutions are heated and generally remove the deposit at
the use of aggressive chemical or mechanical systems that may a slower rate than nitric acid. As the stripping process proceeds,
damage the base material. Consideration of the risk of stripping a corrosion product may form on the surface which will slow
the deposit should always be considered when selecting this the stripping. When this occurs, the steel or copper plated
coating. Undercoats may be required to facilitate rework. The article is removed, rinsed, electrocleaned, rinsed, and returned
commercially available strippers that have minimal attack of to the stripper. As the deposit nears complete removal, it is
the substrate are available to minimize the risk of etching or common for a slight etch of the substrate to occur. The amount
pitting of the substrate. of material removed varies from nothing to 0.0003 in.
X7.2 Nitric acid is recommended to strip electroless nickel
X7.4 Mechanical peening with a grit is effective in remov-
deposits from aluminum. A solution of between 20 % to 30 %
ing electroless nickel from hard steel parts with non-critical
by weight nitric acid should be prepared. After mixing, let
tolerances. The article is placed in a chamber and blasted with
stand until the temperature reaches ambient. If significant area
a heavy grit until all the deposit is removed. This method is
is to be stripped, the solution should be cooled. Articles to be
effective when parts are large and stripping solutions would be
stripped should be clean and free of oils and surface debris that
difficult to manage.
may interfere with the stripping process. Racks and fixtures
made with nylon and drylen are not recommended and are not X7.5 Generally the rework process is limited to less than
compatible with nitric acid and will decompose to a sticky tar
three times. This is because there is some substrate removal
in the stripper. This tar will be difficult to remove from the
each time the article is stripped. When processing some copper
article after stripping. After all the electroless nickel is
or steel alloys, it is advisable to apply a copper undercoat that
removed, the part should be rinsed in clean rinse water.
will prevent the attack of the substrate was the stripping nears
X7.3 Highly alkaline solutions using nitro benzoic acids are completion. This is always a good practice when dealing with
used to remove electroless nickel from steels and coppers. high value copper alloy articles.

X8. WT % P DETERMINATION

X8.1 The following analysis can be used to determine X8.3.4.3 200 mL concentrated nitric acid, HNO3.
weight % P in electroless nickel deposit by means of colori- X8.3.4.4 When ammonium molybdate and ammonium va-
metric methods. The method is also described in Ref (8). nadate solutions are cool, combine together with concentrated
nitric acid and dilute to 1 L total volume in a volumetric flask
X8.2 Samples for testing may be produced by plating an
to the mark.
electroless nickel deposit over a stainless steel, titanium or
aluminum coupon where the surface of the coupon is not X8.4 Analysis Procedure
prepared to produce optimal bonding of the coating to the
substrate. Once the electroless nickel deposit has been applied X8.4.1 Weigh out approximately 200 mg of electroless
on the coupon, the edges of the coupon may be sanded to nickel deposit sample, record sample weight to nearest mg.
remove plated deposit from coupon edges and then the coupon X8.4.2 Working under a fume hood, dissolve electroless
can be bent back and forth as needed, to delaminate the nickel deposit sample in 100 mL of 40 % HNO3 using a hot
electroless nickel as a foil, chips or flakes, or combinations plate. Bring the solution to a boil to completely dissolve the
thereof, from the coupon. The resulting deposit sample (sepa- nickel deposit sample and drive off any brown fumes.
rated from the coupon) is then used for the test. X8.4.3 While solution is boiling, add 25 mL potassium
X8.3 Reagents permanganate solution and allow to boil an additional 5 min. A
brown precipitate of manganese dioxide will form.
X8.3.1 40 % v/v concentrated nitric acid, HNO3.
X8.4.4 Add dropwise 4 % sodium nitrite solution to the
X8.3.2 4 % sodium nitrite solution, NaNO2.
sample until the manganese dioxide precipitate re-dissolves
X8.3.3 0.1 Molar potassium permanganate solution, into the sample.
KMnO4.
X8.4.5 Remove sample from hot plate and allow to cool.
X8.3.4 Molybdate-vanadate solution.
X8.3.4.1 20 g ammonium molybdate tetrahydrate, X8.4.6 Pour cooled sample into a 250 mL volumetric flask
H24Mo7N6O24. 4H2O, dissolved in hot water. and dilute with H2O to the mark.
X8.3.4.2 1 g ammonium metavanadate, NH4VO3, dissolved X8.4.7 Pipet 10 mL of the sample solution into a 100 mL
in hot water (separately from ammonium molybdate). volumetric flask.

15
 B733 − 22
X8.4.8 Pipet 25 mL of molybdate-vanadate solution into the X8.5.2 Dissolve in H2O and then dilute to 1 L exactly using
100 mL volumetric flask containing the sample solution. Dilute a volumetric flask. To determine the amount of phosphorous
the sample with H2O to the mark, mix well, and allow sample (mg) per 1 mL of a 1 L solution, divide the weight of KH2PO4
to develop for 5 min. by (0.4392 g x 0.1 mg).
X8.4.9 Measure the absorbance of the sample at 420 nm
NOTE X8.1—As an example, 0.44 g sample of KH2PO4 diluted to 1 L
using a visible light spectrophotometer. Determine the mg P will result in 0.1002 mg per 1 mL of sample ((0.4400/0.4392) x 0.1 mg).
contained in the sample from a prepared calibration curve.
X8.4.10 Wt % P in the sample is calculated using the X8.5.3 Pipet 2, 4, 6, 8, and 10 mL of the standard phospho-
following formula: rous solution into separate 100 mL volumetric flasks.
~ M p 2 M contr ! X8.5.4 Pipet 25 mL of the molybdate-vanadate solution into
Wp 5 3 2500 (X8.1) each of the flasks, dilute with H2O to the mark, mix well, and
M sample
allow each sample to develop for 5 min. This set of standard-
where:
ized solutions will be used to construct the calibration curve.
Wp = weight % Phosphorous,
Mp = weight (mg) of P in sample from calibration curve, X8.5.5 Measure the absorbance of each sample at 420 nm
Mcontr = weight (mg) of P in control, and using a visible light spectrophotometer. Plot a calibration curve
Msample = weight (mg) of sample. of absorbance vs mg P.
X8.5 Calibration Curve Preparation X8.5.6 Measure the absorbance of a control sample pre-
X8.5.1 Weigh out as close as possible, 0.4392 g of stock pared using all the reagents used in the analysis except without
Potassium dihydrogen orthophosphate (KH2PO4) that has been any sample.
dried thoroughly at 115 °C for 1 h prior to weighing.

REFERENCES

(1) Symposium on Electroless Nickel Plating, ASTM STP 265, ASTM, (5) Mallory, G., and Hajdu, J. “Electroless Plating,” AESF 12644
1959. Research Parkway, Orlando, FL 32826, 1990.
(2) Engineering Properties of Electroless Nickel, The International Nickel (6) Parker, K., “Effects of Heat Treatment on the Properties of Electroless
Co., Inc., New York, NY. Nickel Deposits,” Plating and Surface Finishing, Vol 68, December
(3) Gawrilov, C. G., Chemical (Electroless) Nickel Plating, Portcullis 1981.
Press, London, 1974. (7) Parker, K.,“ Hardness and Wear Resistance Tests of Electroless Nickel
(4) Safranek, W. H., The Properties of Electrodeposited Metals and Deposits,” Plating, Vol 61, September 1974 .
Alloys, The American Electroplaters and Surface Finishers Society, (8) Riedel, W., Electroless Nickel Plating, ASM International, Metals
12644 Research Parkway, Orlando, FL 32826, 1986 Chapter 23. Park, Ohio, 1991, Chapter 7.

SUMMARY OF CHANGES

Committee B08 has identified the location of selected changes to this standard since the last issue (B733 – 21)
that may impact the use of this standard.

(1) Added Appendix X8.

Committee B08 has identified the location of selected changes to this standard since the last issue (B733 – 15)
that may impact the use of this standard.

(1) MIL-R-81841 was cancelled in April 2012. Removed (4) Replaced minimum time requirement for post heat treat-
reference to MIL-R-81841 and replaced with AMS 2590. ment of class 4, 5 and 6 to match time range in Table 3 (4.3.4;
(2) MIL-S-13165 was cancelled in February 1998. Removed 4.3.5; 4.3.6).
reference to MIL-S-13165 and replaced with AMS 2430. (5) Corrected reference in 5.1.4 (was 6.5, should be 6.3).
(3) MIL-STD-105 was cancelled in February 2008. Removed (6) Removed mandatory language from Note 8, moved to new
reference to MIL-STD-105 and replaced with MIL-STD-1916 6.8.3.
or ANSI/ASQ Z1.4. (7) Removed mandatory language from Note 10, moved to 8.2.

16
 B733 − 22
(8) Updated X1.4 Procedure to include refacing CS-10 wheels (10) Updated definition of “A” in X1.5.1 and X1.5.2 as weight
before running test (X1.4.3.1); brushing specimen before of specimen after 1000 cycle break-in period and “B” as weight
weighing (X1.4.3.2) weighing specimen after final abrasion of specimen after final abrasion.
(X1.4.3.5). (11) Corrected X1.6.1 so mean weight loss is reported in
(9) Added Note X1.2. milligrams rather than per 1000 cycles.

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17