British Standard

A single copy of this British Standard is licensed to

Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

BP Coryton ERO
25 November 2002

This is an uncontrolled copy. Ensure use of the most

current version of this document by searching British
Standards Online at bsonline.techindex.co.uk
 BRITISH STANDARD BS 3189:1991
ISO 9717:1990

Method for specifying

Phosphate conversion
coatings for metals
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI
 BS 3189:1991

Committees responsible for this

British Standard

The preparation of this British Standard was entrusted by the Surface

Coatings (other than Paints) Standards Policy Committee (SRC/-) to Technical
Committee SRC/38, upon which the following bodies were represented:

Aluminium Federation
British Metal Finishing Suppliers’ Association
EEA (the Association of Electronics, Telecommunications and Business
Equipment Industries)
Institute of Corrosion
Institute of Metal Finishing
Magnesium Industry Council
Metal Finishing Association
Paintmakers Association of Great Britain Ltd.
Society of Motor Manufacturers and Traders Limited
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

This British Standard, having

been prepared under the
direction of the Surface
Coatings (other than Paints)
Standards Policy Committee,
was published under the
authority of the Standards
Board and comes
into effect on
28 June 1991

© BSI 12-1998
Amendments issued since publication
First published, December 1959
Second edition, September 1973 Amd. No. Date Comments
Third edition, June 1991

The following BSI references

relate to the work on this
standard:
Committee reference SRC/38
Draft for comment 88/56043 DC

ISBN 0 580 19744 1

 BS 3189:1991

Contents

Page
Committees responsible Inside front cover
National foreword ii
1 Scope 1
2 Normative references 1
3 Information to be supplied by the purchaser to the coater 1
4 Coating classification code 1
5 Sampling 2
6 Treatment of basis metals before coating 2
7 Phosphate conversion coating 2
8 Heat treatment after coating 2
9 After treatment 2
Annex A Guidance information 3
Annex B Recommendations for phosphate conversion
coatings to provide corrosion protection 4
Annex C Recommendations for phosphate conversion
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

coatings to ensure good adhesion of paints, varnishes and

related coatings and to improve corrosion resistance 5
Annex D Recommendations for phosphate conversion
coatings to facilitate cold forming 6
Annex E Recommendations for phosphate conversion
coatings to facilitate sliding action 6
Annex F Guidance on heat treatment of steel 6
Annex G Appearance of types of phosphate conversion coatings 7
Annex H Determination of corrosion resistance 8
Annex J Identification of phosphate conversion coatings 9
Table 1 — Summary of principal types of phosphate
conversion coatings 1
Table A.1 — Characteristics of phosphate conversion coatings 4
Table B.1 — Recommendations for phosphate conversion
coatings and after-treatment to provide corrosion protection 5
Table C.1 — Recommendations for phosphate conversion
coatings to ensure good adhesion of painted and related
coatings and to improve corrosion resistance 5
Table D.1 — Recommended zinc phosphate conversion
coating mass per unit area to facilitate cold forming 6
Table E.1 — Recommended manganese phosphate conversion
coating mass per unit area to facilitate sliding action 6
Table F.1 — Hydrogen embrittlement relief after phosphating 7
Table G.1 — Usual appearance of phosphate conversion coatings 8
Table H.1 — Minimum permissible exposure time (in hours)
before first corrosion for non-after-treated, phosphated ferrous
components 8
Table J.1 — Identification of phosphate conversion coating type 9
Publication(s) referred to Inside back cover

© BSI 12-1998 i
 BS 3189:1991

National foreword

This British Standard has been prepared under the direction of the Surface
Coatings (other than Paints) Standards Policy Committee. It is identical with
ISO 9717:1990, “Phosphate conversion coatings for metals — Method of
specifying requirements”, prepared by Subcommittee 8, Conversion coatings, of
Technical Committee 107, Metallic and other inorganic coatings, of the
International Organization for Standardization (ISO), with the active
participation and approval of the UK.
As this standard is based on requirements to be agreed between the
interested parties it is no longer appropriate for any claim to be made
that a coating complies with this British Standard.
As stated above, this revision of BS 3189 differs from the 1973 edition in that it
has been written in the form of a method for specifying, rather than a
specification. The standard has also been extended to cover not only phosphate
coatings on ferrous metals but also on aluminium, zinc, cadmium and their alloys.
However, this revision does not include appendices containing methods of test as
these are now published separately as Parts of BS 5411 and BS 5466. With the
publication of this revision, BS 3189:1973 is withdrawn.
Additional information
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

Phosphate conversion coatings are applied to ferrous metals, aluminium, zinc,

including zinc plated steel, cadmium and their alloys, either as an end finish or
as an intermediate layer for other coatings.
They are intended to:
a) impart corrosion resistance;
b) improve adhesion to paints and other organic finishes;
c) facilitate cold forming operations such as wire drawing, tube drawing and
extrusion;
d) modify surface frictional properties so as to facilitate sliding.
A general description of the principal processes is given for guidance in annex A.
Recommendations for coating and after-treatment for each end use are given in
annex B, annex C, annex D and annex E.

Cross-references
International standard Corresponding British Standard
ISO 3768:1976 BS 5466 Methods for corrosion testing of metallic
coatings
Part 1:1977 Neutral salt spray test (NSS test)
(Identical)
ISO 3892:1980 BS 5411 Methods of test for metallic and related
coatings
Part 14:1982 Gravimetric method for determination of
coating mass per unit area of conversion coatings on
metallic materials
(Identical)
ISO 4519:1980 BS 6041:1981 Method of sampling of electrodeposited
metallic coatings and related finishes: procedures for
inspection by attributes
(Identical)

ii © BSI 12-1998
 BS 3189:1991

A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

Summary of pages
This document comprises a front cover, an inside front cover, pages i to iv,
pages 1 to 10, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on
the inside front cover.

© BSI 12-1998 iii

Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

iv
blank
 ISO 9717:1990(E)

1 Scope i) the requirement for corrosion resistance

This International Standard describes a method of
specifying requirements for phosphate conversion
coatings, intended primarily for application to
ferrous metals, aluminium, zinc, cadmium and their
alloys.
2 Normative references
The following standards contain provisions which,
through reference in this text, constitute provisions
of this International Standard. At the time of
publication, the editions indicated were valid. All
standards are subject to revision, and parties to
agreements based on this International Standard
are encouraged to investigate the possibility of
applying the most recent editions of the standards
indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI
(see 7.3 and annex H).
3.2 Additional information
The following additional information may be
required and, if so, shall be specified by the
purchaser, if necessary in consultation with the
coater:
Any requirements for stress relieving treatment
before phosphating and/or hydrogen embrittlement
reduction after phosphating (see annex F).
4 Coating classification code
4.1 Types of coating
The principle types of phosphate conversion
coatings and their designations are given in Table 1.
Table 1 — Summary of principle types of
phosphate conversion coatings

ISO 3768:1976, Metallic coatings — Neutral salt Coating type Designation

spray test (NSS test). Zinc phosphate Znph
ISO 3892:1980, Conversion coatings on metallic Zinc-calcium phosphate ZnCaph
materials — Determination of coating mass per unit Manganese phosphate Mnph
area — Gravimetric methods.
Iron(II) phosphate Fehph
ISO 4519:1980, Electrodeposited metallic coatings Iron(II) phosphated (produced by
and related finishes — Sampling procedures for Feph
alkali-metal phosphate treatment)
inspection by attributes.
NOTE 2 Other coating types exist including zinc phosphate
modified with iron and/or nickel and/or manganese. The
3 Information to be supplied by the modifying metal will normally be present in the form of a double
purchaser to the coater salt such as Zn2Me(PO4)2.4H2O, where Me represents Fe(II), Ni
or Mn. Zinc remains the main metal constituent of these coatings
NOTE 1 Close liaison between designers, manufacturers and which, to avoid confusion, have not been given separate
conversion coaters is necessary to obtain satisfactory conversion designations. It should also be noted that metal from the
coatings and to avoid adverse effects on the mechanical substrate material will often be incorporated in the conversion
properties of the article. coating.
3.1 Essential information 4.2 Conversion coating classification code
The following information shall be supplied by the The coating classification code comprises the
purchaser to the conversion coater: following four elements.
a) the number of this International Standard a) A symbol given in Table 1, which is the
i.e. ISO 9717; designation of the type of coating;
b) the nominal composition or specification and b) A symbol indicating the function of the
metallurgical condition of the basis material; conversion coating, as follows:
c) the sampling procedure to be adopted and r — corrosion protection;
acceptable quality levels (AQL’S) required
z — to facilitate cold forming;
(see clause 5);
g — to facilitate sliding action.
d) the coating classification code (see clause 4);
e) the coating mass per unit area (see 7.2) and, if c) A number indicating the coating mass per unit
agreed, the coating thickness (see 7.2, note 5) area, in grams per square metre, with a tolerance
of ± 30 %.
required;
d) A symbol indicating any after-treatment of the
f) any requirements for after-treatment
conversion coating, as follows:
[see 4.2 d)];
e — dyeing;
g) the surface preparation required prior to
phosphate conversion coating f — application of grease or oil;
(see annex A, clause A.2); w — application of wax;
h) the surface appearance (see 7.1); s — application of soap;

© BSI 12-1998 1
 ISO 9717:1990(E)
a — application of paints, varnishes or similar
coating materials;
d — application of inorganic or non
film-forming organic sealants.
The conversion coating classification code, which is
appended to the designation of the basis metal of the
components to be phosphated, will not necessarily
contain the four elements, for example only three
elements would be needed if no after-treatment is
required. Combinations of after-treatment may be
employed, for example dyeing c), followed by
oiling f) or sealing d), followed by painting a).
An example of a complete phosphate
conversion coating classification code is as
follows:
A zinc phosphate type coating applied to give
corrosion protection at a mass per unit area
of 3 g/m2 ± 0,9 g/m2 and for which the
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI
after-treatment is painting, has the coating
classification number
Znph r 3 a
5 Sampling
Samples for test purposes shall be selected in
accordance with the appropriate procedures given in
ISO 4519.
These samples shall be of the same metal or alloy as
the components that they represent, and shall
possess similar surface characteristics to them.
6 Treatment of basis metals before
coating
6.1 Stress relief
If the purchaser specifies that stress relief
treatment is required (see 3.2) the necessary heat
treatment should be carried out in accordance with
annex F, clause F.1.
6.2 Shot peening
See annex F, clause F.1.
7 Phosphate conversion coating
7.1 Appearance
Inspection of the surface should be in accordance
with the information given in annex G, to evaluate
the appearance (colour and crystal size) and
uniformity of the coatings.
7.2 Coating mass per unit area
The coating mass per unit area should be in
accordance with the appropriate recommendations
given in annex B, annex C, annex D and annex E
and shall be determined in accordance with the
appropriate method specified in ISO 3892.
2 © BSI 12-1998
NOTE 3 For quality assurance purposes, instruments which
are available and which give a direct reading of coating mass per
unit area may be used. It is, however, essential that they be
calibrated against standard coatings having coating mass per
unit area of the same order as those being inspected.
NOTE 4 If required, the type of coating used may be identified
by means of the method specified in annex J.
NOTE 5 If the case of heavy coatings, the amount of phosphate
deposited is sometimes expressed in terms of coating thickness,
particularly for quality control purposes. The use of this
alternative (and selection of a relevant test method) should be a
matter for agreement between the purchaser and the coater.
NOTE 6 Other properties of the coating such as surface profile
and crystal size may be specified as an agreement between the
purchaser and the coater.
7.3 Corrosion resistance
The corrosion resistance of the coated component
should be determined using the appropriate
procedure specified in annex H.
7.4 Suitability of coating to facilitate cold
forming
Test methods to determine the suitability of a
phosphate conversion coating to facilitate cold
forming are not specified because of the difficulty of
simulating actual processing conditions. Selection of
the appropriate coating should therefore be in
accordance with the recommendations given in
annex D.
7.5 Suitability of coating to facilitate sliding
action
Test methods to determine the suitability of a
phosphate conversion coating to facilitate sliding
action are not specified because of the difficulty of
simulating actual processing conditions. Selection of
the appropriate coating should therefore be in
accordance with the recommendations given in
annex E.
8 Heat treatment after coating
If the purchaser specifies that hydrogen
embrittlement relief is required (see 3.2), the
necessary heat treatment should be carried out in
accordance with annex F, clause F.2.
9 After treatment
If the purchaser specifies that after-treatment of the
phosphate coated surface is required [see 3.1 f)] the
necessary treatment should be carried out in
accordance with the appropriate requirements of
annex B, annex C, annex D and annex E.

Annex A (informative)
Guidance information
A.1 General
Phosphate conversion coatings are produced by
treatment with solutions, the main constituents of
which are the appropriate dihydrogen
orthophosphates shown in Table A.1. These coatings
are applied principally to ferrous materials,
aluminium, zinc and cadmium and differ in coating
mass per unit area and apparent density, depending
on
a) the construction material and surface
condition of the components;
b) previous mechanical and chemical treatment
of the components;
c) processing conditions for phosphating.
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI
NOTE 7 All phosphate conversion coatings are more or less
porous but can be substantially sealed by appropriate
after-treatment.
The main types of phosphate conversion coatings
and their characteristics are summarized in
Table A.1.
A.2 Surface preparation
A.2.1 Before processing, all scale, rust, grease, oil,
finger prints and foreign matter should be removed
from the surface to be coated by a method, or
combination of methods, suitable for the particular
phosphating process concerned, i.e. methods which
give rise to a coarse crystalline structure may not be
desirable. To avoid a phosphate conversion coating
of coarse grain size or excessive coating mass per
unit area, the use of strong alkalies or acids for
cleaning should be minimized. If the conditions of
components require such cleaning prior to
phosphating, a neutralizing rinse should be used.
The cleaned component should be adequately rinsed
in cold or hot water to remove any residues from the
cleaning process which might affect the composition
of the bath solution or the quality of the coating. A
conditioning rinse may be used immediately prior to
phosphating to favour the formation of fine grain
coatings without further rinsing. Materials based on
titanium salts are currently used and are widely
available from proprietary sources. It is also
possible to incorporate such materials in mildly
alkaline spray cleaners, thus obviating the need for
a separate conditioning rinse. However, in this case
rinsing before phosphating is essential.
© BSI 12-1998
ISO 9717:1990(E)
NOTE 8 Certain phosphating processes combine surface
preparation with phosphating.
A.2.2 Where acid pickling has been employed, it
may be necessary to follow the use of pickling
solutions containing wetting agents or inhibitors, by
dipping in an acid solution without wetting agent or
inhibitor or by dipping in a suitable alkaline
solution in order to remove absorbed films.
A.3 Methods of application
Phosphating is usually carried out by immersing the
component in a coating bath (with agitation of the
solution if necessary), or by copious application or
spraying of the component with the coating solution.
Roller application may however be used in the case
of galvanized or ungalvanized steel strip. The
phosphated components are then rinsed with water,
dried and after-treated according to their intended
end use. Full details of the process conditions may,
of course, be obtained from the appropriate
operating instructions.
NOTE 9 Sludge is formed as a normal by-product of the
phosphating reaction. The sludge does not usually interfere with
processing but forms of agitation, which cause sludge to be
deposited on the component, should be avoided. Filtration of the
bath prevents sludge deposition on the work pieces.
Recommendations for the phosphate conversion
coating and after-treatment of ferrous metals,
aluminium, zinc and cadmium in respect of
— corrosion protection;
— improving the adhesion of paints, varnishes
and related coatings and the corrosion resistance
of the basis metal;
— facilitating cold forming;
— facilitating sliding action;
are given in annex B, annex C, annex D and
annex E. respectively.
A.4 Heat treatment after phosphating
See annex F, clause F.2.
3
 ISO 9717:1990(E)

Table A.1 — Characteristics of phosphate conversion coatings

Main Coating mass per unit area (g/m2) on
constituent(s) Coating type Designation Usual appearance of
of phosphating produced of coating coating Ferrous
materials Aluminium Zinc Cadmium
bath

Zn(H2PO4)2 Zinc Light grey to dark

Znph 1 to 30 0,3 to 10 1 to 60 1 to 60
phosphate grey, crystalline
Zn(H2PO4)2 Light grey to dark
Zinc-calcium
ZnCaph grey, finely 1 to 10 — 1 to 10 —
Ca(H2PO4)2 phosphate
crystalline
Mn(H2PO4)2 Manganese Light grey to dark
Mnph 1 to 30 — — —
phosphate grey, crystalline
Amorphous
Phosphate coatings of about
of treated 0,1 g/m2 to 1 g/m2
metal (plus Iridescent
oxides of e.g. yellowish to
Me(I)H2PO4a Feph 0,1 to 1,5 < 0,3 0,1 to 2 —
iron in the bluish grey
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

case of
ferrous Coatings over
materials) about 1 g/m2
Grey
Fe(H2PO4)2 Iron(II) Dark grey,
Fehph 5 to 60 — — —
phosphate crystalline
a
Me(I) denotes cation of alkali metal or NH +4 .

Annex B (informative) In the absence of after-treatment, phosphate

Recommendations for phosphate conversion coatings provide corrosion protection of
only short duration. If the period of protection is to
conversion coatings to provide be extended, additional treatments appropriate to
corrosion protection the end use of the phosphated surface are necessary
Recommandations for phosphate conversion e.g. the application of corrosion-protecting oils,
coatings and after-treatment to provide corrosion greases or waxes (see Table B.1). Such
protection are summarized in Table B.1. after-treatment should preferably be carried out
prior to longer term storage of the phosphated
Phosphate conversion coatings for corrosion
components.
protection are usually given a final rinse with
aqueous solutions containing chromium or certain
organic compounds, such as tannins. Where a
water-soluble organic finish is to be applied without
intermediate drying, a final rinse with de-ionized
water is recommended.

4 © BSI 12-1998
 ISO 9717:1990(E)

Table B.1 — Recommendations for phosphate conversion coatings and after-treatment to

provide corrosion protection
Phosphate coating
Basis Preferred Coating mass per Corrosion protection Typical applications and
After treatment
metal type of unit area effect obtained end uses
treatment
g/m2
Feph 0,1 to < 1,5 None Temporary protection Short term, in-plant
Znph 1 to 5 None in dry environment (no storage of machine
condensation) components (< 24 h)
Znph  None Longer term protection Longer term, in-plant
 > 5 but in dry environment (no storage of machine
 condensation) components (< 7 days)
Mnph  preferably > 10 None
Ferrous 
materials
Znph  Long term protection
 > 5 but Protective oils in dry environment (no
Fehph  preferably > 10 or waxes as
 condensation) Corrosion protection in
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

 required, after transit during long

Mnph dyeing of the Temporary protection term storage
coating outdoors but with
ZnCaph >5 overhead cover

Annex C (informative) If phosphated components are to be painted,

Recommendations for phosphate varnished or similarly coated, they should first be
rinsed in clean tap water and then preferably in
conversion coatings to ensure good demineralized water, so as to ensure that the
adhesion of paints, varnishes and surfaces are free from any water-soluble residues
related coatings and to improve from previous processing etc., which could give rise
corrosion resistance to blister formation in the applied film. It is equally
important that the phosphated surface to be painted
Recommendations for phosphate conversion should be free of additional contamination such as
coatings to ensure good adhesion of paint, varnishes dust or finger prints.
and related finishes, and to improve corrosion
resistance of the basis metal, are summarized in
Table C.1.
Table C.1 — Recommendations for phosphate conversion coatings to ensure good adhesion of
painted and related coatings and to improve corrosion resistance
Phosphate coating
Preferred Coating mass per
Basis metal After-treatment Typical applications and end uses
type of unit area
treatment
g/m2
Ferrous materials
Zinc Znph  1 to 10, but Motor vehicle bodies,
 preferably 1 to 4
Aluminium ZnCaph  refrigerator and washing
Cadmium machine cabinets
Paints, varnishes
Ferrous materials Feph 0,1 to < 1 and related coatings
Motor vehicle bodies, sheets
and strips which are formed
Zinc Znph 1 to 5 after painting and in particular
where flexing of an organic
after-treatment is involved

© BSI 12-1998 5
 ISO 9717:1990(E)

Annex D (informative) b) The coating level used depends on the

Recommendations for phosphate dimensional tolerances of the coated components
in the assembled unit.
conversion coatings to facilitate cold
c) Such coatings are normally used in conjunction
forming with a suitable lubricant.
Zinc phosphate conversion coatings are preferred to Table E.1 — Recommended manganese
facilitate cold forming. Recommendations for phosphate conversion coating mass per unit
coating mass per unit area for various end uses are area to facilitate sliding action
given in Table D.1.
Coating
Zinc phosphate coatings shall be neutralized, after mass per
End use unit area Notes
rinsing, by treatment with a weakly alkaline
aqueous solution. Soap lubrication can take place by g/m 2

dipping in a suitable soap solution (tube drawing, Components with Coating mainly
cold heading and cold extrusion, deep drawing) or small clearances manganese
with dry soap powder (wire drawing). In the case of 3 to 5
e.g. pistons of phosphate
dip application, the soap will react with the zinc
refrigerator (no iron in bath)
phosphate layer, giving rise to zinc stearate on top
compressors
of the zinc phosphate coating. Prior to dry soap
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

lubrication, wires may be immersed in a strong Components with Coating of

solution of borax, lime or sodium metasilicate which
acts as a lubricant carrier.
Table D.1 — Recommended zinc phosphate
conversion coating mass per unit area to
facilitate cold forming
Coating mass
End use per unit area
g/m2
Drawing of steel wire 5 to 15
Drawing of welded steel tubes 3 to 10
Drawing of steel precision tubes 4 to 10
Cold heading and cold extrusion 5 to 20
Deep drawing without wall 2 to 5
thickness reduction
Deep drawing with wall thickness 5 to 15
reduction
Annex E (informative)
Recommendations for phosphate
conversion coatings to facilitate
sliding action
Manganese phosphate coatings are generally
preferred to facilitate sliding action.
Recommendations for such coating mass per unit
area for various end uses are given in Table E.1.
The following factors should also be taken into
consideration.
a) Although manganese phosphate coatings are
generally preferred, other types of coatings, for
example zinc phosphate, are also suitable,
particularly at lower coating levels. The type of
coating selected will depend on the stresses in the
coating involved for the intended end use.
large clearances manganese and
e.g. gears, crown iron phosphates
5 to 20
wheel and pinions (iron present in
of gear units and bath)
differentials
Annex F (informative)
Guidance on the heat treatment of
steel
F.1 Stress relief before phosphating
F.1.1 General
The relief of internal and deleterious surface
stresses by suitable heat treatment aids resistance
to sustained load and fatigue failure. As a rule,
internal stresses developed during quenching are
relieved at temperatures of 400 °C and above, and
surface stresses developed during mechanical
finishing operations can be reduced by heating at
temperatures of 200 °C and above. The relief of
beneficial surface compressive stresses introduced
during production e.g. by shot-peening or surface
rolling should, however, be avoided. Parts may, if
necessary, be degreased before heat treatment but
stress relief should be applied before cleaning. The
stress relief treatment may be omitted for maraging
steels which have been aged after final machining.
F.1.2 Severely cold worked steel parts
Severely cold worked steel parts may require stress
relief. As a guide, the parts should be maintained
for 30 min at the highest temperature which can be
applied without affecting their strengths.

6 © BSI 12-1998

F.1.3 Parts made from steels of tensile strength
in the range 1 000 N/mm2
to 1 400 N/mm2
Parts made from steel of minimum specified tensile
strength of not less than 1 000 N/mm2 (or of
equivalent surface hardness) nor more
than 1 400 N/mm2, which have been ground or
subjected to heavy machining after final tempering,
should be stress relieved at a temperature
between 130 °C and 230 °C (preferably near the
higher end of this range) for not less than 1 h, or to
just below the tempering temperature for
between 5 min and 30 min. Any stress relieving
treatment should be applied after thorough
degreasing and the subsequent complete removal of
the degreasing medium before heating. Parts which
have been treated in order to introduce beneficial
compressive stresses into any part of the surface,
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI
e.g. by shot-peening or cold working, should not be
heated above 130 °C.
F.1.4 Parts made from steels of tensile strength
over 1 400 N/mm2
The standard stress relief consists in heating the
parts to the highest temperature possible within the
limit imposed by the tempering or ageing
temperature or by any susceptibility of the steel to
temper brittleness, and in any case to not less
than 200 °C. The period at this temperature should
be not less than either 18 h at 200 °C, 6 h
at 250 °C, 2 h at 300 °C or 1 h at 400 °C or above,
followed by cooling in still air. Case hardened parts
which are not to be phosphated on the hardened
area may, however, be stress relieved at only 130 °C
for 6 h, as a higher temperature may reduce the
hardness of the case to an unacceptable degree.
The above standard stress relief procedure should
be applied to all parts which have not been given a
mechanical treatment to introduce beneficial
compressive stresses into the surface e.g. by
shot-peening or surface rolling.
Standard stress relieving prior to treatments given
to introduce beneficial compressive stresses into the
surface is recommended and, if applied, should not
be repeated after the mechanical treatment. If no
prior stress relief is applied, then parts given a
mechanical treatment all over should not be stress
relieved after treatment and parts given a
mechanical treatment over only part of the surface
should be subsequently stress relieved by the
standard procedure but at a temperature within the
range 200 °C to 230 °C.
NOTE 10 Notwithstanding the above, shot-peened or vapour
blasted springs may be stress relieved at any temperature up
to 230 °C.
© BSI 12-1998
ISO 9717:1990(E)
F.2 Hydrogen embrittlement relief after
phosphating
F.2.1 Severely cold worked steels
Parts made from severely cold worked steels or from
steels of tensile strength of about 1 000 N/mm2 or
greater should be heat treated immediately after
phosphating, rinsing and drying, and before
application of the supplementary finish. The
conditions of heat treatment are given in Table F.1.
NOTE 11 Attention is drawn to the possible dehydration of
phosphate coatings, particularly those of zinc phosphate, and
consequent lowering of corrosion resistance by de-embrittlement
at the higher temperatures. Preferably, zinc phosphate coatings
should not be heated above 150 °C and manganese phosphate
coatings not above 170 °C.
F.2.2 Surface-hardened steels
Steels which have been carburized, flame hardened
or induction hardened and subsequently ground
would be adversely affected by the treatment given
in Table F.1 and should instead be heat treated at a
lower temperature, for example at 130 °C to 150 °C
for not less than 6 h.
Table F.1 — Hydrogen embrittlement relief
after phosphating
Tensile strength
Heat treatment
N/mm2
1 000 to 1 400 130 °C to 200 °C for 1 h
minimum
1 400 to 1 800 150 °C to 200 °C for 4 h
minimum
Greater than 1 800 170 °C to 200 °C for 6 h
minimum
NOTE The temperatures referred to are those of the part.
Annex G (informative)
Appearance of types of phosphate
conversion coatings
The usual appearance (crystallinity, colour and
uniformity of coating) of the principle types of
phosphate conversion coatings is summarized in
Table G.1.
Grain size may be determined by use of an optical or
scanning electron microscope.
The phosphate layer should be uniform, free from
spots, uncoated areas, scratches, powder and white
residues. Differences in colour or shade in different
areas or from piece to piece should not be considered
as causes for rejection.
Minor variations in the appearance of phosphate
coatings caused, for example, by variations in the
surface of the basis material or by contact with
racks during phosphating are common and are not
normally indicative of important fluctuations in
performance.
7
 ISO 9717:1990(E)

Table G.1 — Usual appearance of phosphate conversion coatings

Coating type How viewed Colour Crystallinity Uniformity of coating

Znph Light grey to dark

grey Crystalline
Mnph Unaided vision or
structure usually
Fehph magnification < × 6 Fehph coatings are
observable
dark grey
Finely crystalline Uniform coating, no
Znph Crystalline trace of white spots,
Light grey to dark
Magnification < × 6 structure hardly corrosion products
Mnph grey
observable or finger print
ZnCaph traces
Iridescent ranging
from yellowish to
bluish grey (for coating
2 No crystalline
Feph Magnification < × 6 levels ≈ 0,1 g/m
2
to 1 g/m ) structure observable
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

Grey (for coating

levels > ≈ 1 g/m2)

Annex H (informative) H.2 Determination of corrosion resistance of

Determination of corrosion resistance phosphate conversion coatings which have
been after-treated with corrosion-preventing
H.1 Determination of corrosion resistance of oils
phosphate coated metals which have not been H.2.1 Principle
after-treated or organically coated
Phosphated test pieces are after-treated with the
Use the procedure specified in ISO 3768. appropriate corrosion-protecting medium under
The phosphated components or test panels to be specified conditions and these after-treated test
examined are placed in the test cabinet, exposed to pieces are subjected to the neutral salt spray (NSS)
the specified environment during the periods stated test described in ISO 3768. The test may be used
in Table H.1, and removed for evaluation. either to evaluate a specific corrosion-protecting
system or for comparative testing of a range of
Table H.1 gives the minimum exposure times, in
phosphate conversion coatings in conjunction with a
hours, which have to be attained by
specific corrosion-preventing oil.
non-after-treated, phosphated ferrous components
before the first evidence of corrosion appears. H.2.2 After-treatment
Table H.1 — Minimum permissible exposure H.2.2.1 Specific treatment
time (in hours) before first corrosion for Immerse the phosphated component or test panel in
non-after-treated, phosphated ferrous the corrosion-protecting medium under
components examination, following carefully the appropriate
Type of Zinc Manganese Iron(II) instructions and ensuring that the liquid, semi-solid
phosphate phosphate phosphate phosphate or waxy film which is thereby formed on the
coating coatings coatings coatings
phosphated surface is free from air bubbles and
Classification Znph Mnph Fehph discontinuities.
code Before testing, suspend the test pieces for at
Coating mass > 10 > 15 > 15 least 24 h at a temperature of 23 °C ± 5 °C and a
per unit area relative humidity not exceeding 65 %, in a dust and
(g/m2) draught-free atmosphere, so as to allow the surplus
of oil to drip off and the solvents to evaporate.
Minimum 2 1,5 1,5
exposure
time (h)

8 © BSI 12-1998

H.2.2.2 Comparative testing
Suspend the phosphated test pieces (previously
dried at a temperature of between 100 °C
and 120 °C and cooled to room temperature) from
suitable plastics hooks or plastics-coated steel hooks
and immerse them vertically in the selected oil
for 1 min at a temperature of 25 °C ± 2 °C. During
this time, move the test panels gently to and fro and
then withdraw them gradually from the oil in
about 30 s. The oil film so formed on the phosphated
surface shall be free from air bubbles and
discontinuities.
Suspend the test panels for at least 24 h at a
temperature of 23 °C ± 5 °C and a relative humidity
not exceeding 65 %, in a dust and draught-free
atmosphere, prior to testing.
H.2.3 Procedure
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI
Subject the after-treated components or test panels
(see H.2.2) to the neutral salt spray test described in
ISO 3768.
NOTE 12 This test determines the exposure times attainable by
a specific corrosion-protecting system before the first evidence of
corrosion becomes visible.
For this purpose, take test pieces from the test chamber at
predetermined intervals and examine them visually for evidence
of corrosion. By special agreement, it may be specified whether or
not the after-treatment film (or layer) is to be removed before
visually examining the components or test panels.
For a specific phosphate coating, considerable
scatter occurs in the exposure times up to the first
occurence of corrosion, depending on the
composition of the after-treatment medium and the
coating level. The specifying of minimum exposure
times for after-treated phosphate conversion
coatings shall therefore always be referred to a
specific product from the category of
corrosion-preventing oils, greases and waxes, of
known coating level, in grams per square metre, as
determined by mass difference.
NOTE 13 The minimum exposure-time and mode of assessment
should be agreed between the parties.
Annex IJ (informative)
Identification of phosphate
conversion coatings
J.1 Scope
This annex describes methods for identifying the
type of phosphate conversion coating. They are
applicable to coatings containing phosphorus, iron,
manganese, zinc and calcium. They are not
applicable to the detection of iron or zinc if these
metals are present in the basis material.
© BSI 12-1998
ISO 9717:1990(E)
J.2 Method 1
J.2.1 Principle
Removal of the phosphate conversion coating from a
test specimen by treatment with sodium hydroxide
solution. Detection of the elements present in the
solution by any suitable instrumental analytical
technique e.g. atomic absorption spectrometry.
J.2.2 Reagents
During the analysis, use only reagents of recognized
analytical grade and distilled water, or water of
equivalent purity.
J.2.2.1 Sodium hydroxide, approximately 50 g/l
solution.
J.2.3 Apparatus
Ordinary laboratory apparatus, and
J.2.3.1 Any appropriate instrument, suitably
equipped for the detection of phosphorus,
manganese, zinc and calcium e.g. an atomic
absorption spectrometer for metals.
J.2.4 Test specimen
Use a test specimen having a total coated surface
area of approximately 100 cm2.
J.2.5 Procedure
Immerse the test portion (J.2.4) in 100 ml of the
sodium hydroxide solution (J.2.2.1) maintained at a
temperature of 80 °C to 90 °C, until the coating has
been removed or has at least undergone obvious
attack. If necessary, remove the coating by rubbing
with a rubber squeegee. Using the appropriate
analytical instrument (J.2.3.1), detect which of the
elements, phosphorus, manganese, zinc and
calcium, are present in the test solution.
J.3 Method 2
As an alternative to method 1 (clause J.2) a
scanning electron miscroscope equipped for Energy
Dispersive Spectroscopy (EDS) may be used for the
direct detection of metal elements in the coating.
J.4 Interpretation of results
Taking account of the elements detected, identify
the types of coating in accordance with Table J.1.
Table J.1 — Identification of phosphate
conversion coating type
Elements detected Coating type
Phosphorus Phosphate
Manganese Mnph
Zinc (no calcium) Znph
Zinc and calcium ZnCaph
For ferrous basis materials, the absence of
manganese or zinc in the conversion coating
indicates almost certainly that the coating consists
of iron(II) phosphate.
9
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

10
blank
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

© BSI 12-1998
See national foreword.
Publication(s) referred to
BS 3189:1991
 |
|
|
|
|
|
|
|
|
BSI Ð British Standards Institution
|
|
|
|
|
|
| BSI is the independent national body responsible for preparing British Standards. It
|
| presents the UK view on standards in Europe and at the international level. It is
| incorporated by Royal Charter.
|
|
| Revisions
|
|
| British Standards are updated by amendment or revision. Users of British Standards
|
| should make sure that they possess the latest amendments or editions.
|
|
| It is the constant aim of BSI to improve the quality of our products and services. We
|
| would be grateful if anyone finding an inaccuracy or ambiguity while using this
| British Standard would inform the Secretary of the technical committee responsible,
|
| the identity of which can be found on the inside front cover. Tel: 020 8996 9000.
|
| Fax: 020 8996 7400.
|
|
| BSI offers members an individual updating service called PLUS which ensures that
|
| subscribers automatically receive the latest editions of standards.
|
|
| Buying standards
|
| Orders for all BSI, international and foreign standards publications should be
|
| addressed to Customer Services. Tel: 020 8996 9001. Fax: 020 8996 7001.
Licensed Copy: BP Coryton ERO, BP Amoco, 25 November 2002, Uncontrolled Copy, (c) BSI

|
|
| In response to orders for international standards, it is BSI policy to supply the BSI
|
| implementation of those that have been published as British Standards, unless
|
| otherwise requested.
|
|
| Information on standards
|
| BSI provides a wide range of information on national, European and international
|
| standards through its Library and its Technical Help to Exporters Service. Various
|
| BSI electronic information services are also available which give details on all its
|
| products and services. Contact the Information Centre. Tel: 020 8996 7111.
|
| Fax: 020 8996 7048.
|
|
| Subscribing members of BSI are kept up to date with standards developments and
| receive substantial discounts on the purchase price of standards. For details of
|
| these and other benefits contact Membership Administration. Tel: 020 8996 7002.
|
| Fax: 020 8996 7001.
|
|
| Copyright
|
|
| Copyright subsists in all BSI publications. BSI also holds the copyright, in the UK, of
|
| the publications of the international standardization bodies. Except as permitted
| under the Copyright, Designs and Patents Act 1988 no extract may be reproduced,
|
| stored in a retrieval system or transmitted in any form or by any means ± electronic,
|
| photocopying, recording or otherwise ± without prior written permission from BSI.
|
|
| This does not preclude the free use, in the course of implementing the standard, of
|
| necessary details such as symbols, and size, type or grade designations. If these
|
| details are to be used for any other purpose than implementation then the prior
| written permission of BSI must be obtained.
|
|
| If permission is granted, the terms may include royalty payments or a licensing
|
| agreement. Details and advice can be obtained from the Copyright Manager.
|
| Tel: 020 8996 7070.
|
|
|
|
|
|
|
|
|
BSI |
|
389 Chiswick High Road |
|
London |
|
W4 4AL |
|
|
|
|
|
|