Ministry of Defence

Defence Standard

03-11/Issue 3 24 February 1995

PHOSPHATE TREATMENT OF
IRON AND STEEL

This Defence Standard supersedes

Def Stan 03-11/Issue 2
dated 26 May 1986
DEF STAN 03-11/3

AMENDMENTS ISSUED SINCE PUBLICATION

AMD NO DATE OF TEXT AFFECTED SIGNATURE &

ISSUE DATE

Revision Note
This Defence Standard has been based on the requirements of Def Stan
03-11/2 but with layout to Def Stan 00-00 Part 2.
Historical Record
DEF-29A dated September 1965
Def Stan 03-11 Issue 1 dated 21 November 1974
Def Stan 03-11 Issue 2 dated 26 May 1986
 DEF STAN 03-11/3

PHOSPHATE TREATMENT OF IRON AND STEEL

PREFACE

This Defence Standard supersedes

Def Stan 03-11/2 dated 26 May 1986

i This Defence Standard specifies requirements for the Phosphate Treatment

of Iron and Steel.
ii This Standard has been produced on behalf of the Defence Engineering
and Equipment Standardization Committee (DEESC) by the Corrosion Prevention
of Metals Subcommittee (E3) and has been agreed by the authorities
concerned with its use and is intended to be used whenever relevant in all
future designs, contracts, orders etc and whenever practicable by amendment
to those already in existence. If any difficulty arises which prevents
application of the Defence Standard, the Directorate of Standardization
shall be informed so that a remedy may be sought.
iii Any enquiries regarding this Standard in relation to an invitation to
tender or a contract in which it is incorporated are to be addressed to the
responsible Technical or Supervising Authority named in the invitation to
tender or contract.
iv This Standard has been devised for the use of the Crown and of its
contractors in the execution of contracts for the Crown. The Crown hereby
excludes all liability (other than liability for death or personal injury)
whatsoever and howsoever arising (including, but without limitation,
negligence on the part of the Crown its servants or agents) for any loss or
damage however caused where the Standard is used for any other purpose.

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PAGE
CONTENTS
1
Preface
Section One. General
0 Introduction 3
1 Scope 4
2 WARNING 4
3 Related Documents 4
4 Definitions 5
5 Information to be Supplied to the Processor 6
6 Process Control 7

Section Two. Process Requirements

7 General 8
8 Heat Treatment 8
9 Surface Preparation 8
10 Phosphate Treatment 8
11 Washing 9
12 Staining 9
13 Drying 10
14 Heat Treatment Relief of Hydrogen Embrittlement 10
15 Sealing 10

Section Three. Inspection and Test

16 Inspection 11
17 Selection of Test Samples 11
18 Visual Inspection 11
19 Test for the Presence of a Coating 11
20 Coating Weight 12
21 Freedom from Corrosive Residues 12
22 Resistance to Salt Spray 12
23 Re-treatment of Items Rejected on Inspection 13

Table A Tensile Strength of Steels 6

Table B Coating Weight 12
Table C Examples of Supplementary Finishes for Resistance to 13
Salt Spray
Table D Loss in Weight of Control Specimens E-3

Figure E.1 Test Panel E-1

Annex A Determination of Rinse Water Contamination A-1

Annex B Phosphating of High Strength Steels B-1
Annex C Determination of Phosphate Coating Weight C-1
Annex D Determination of the Freedom from Corrosive Residues D-1
Annex E Salt Droplet Test E-1
Annex F Approximate Conversion of Metric Units to Imperial F-1
Equivalents

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PHOSPHATE TREATMENT OF IRON AND STEEL

Section One. General

0 Introduction
This document constitutes the requirements for the phosphate treatment of
iron and steel to provide coatings for the protection of items against
corrosion and wear. It covers four classes of phosphate coatings, which
are designated as follows:

Class I - A coating consisting essentially of inorganic phosphates

2
of
manganese or iron and having a weight of not less than 7.5 g/m of treated
surface. The coating is produced by certain immersion-type accelerated and
unaccelerated processes. This class will be used normally when sealing
with oil or grease supplementary finishes are specified, and maximum
corrosion protection (or wear resistance) is desired. It is not
recommended for use under paint, varnish, and lacquer finishes on sheet
materials less than 1.0 mm thick.
Class II – A coating consisting essentially of
2
inorganic phosphates of zinc
and having a weight of not less than 4.5 g/m of treated surface. The
coating is usually produced by an immersion-type accelerated process. This
class will normally be used for general protective purposes under paint
finishes. A Class I coating may be used when a Class II coating is called
for, except on thin sheet materials.
Class III - A coating consisting essentially of inorganic phosphates
2
of
zinc or iron and having a weight within the range 1.5 to 4.5 g/m of
treated surface. The coating is usually produced by a spray-type
accelerated process. This class will normally be used only for the
pre–treatment of thin sheet steel sections under paint, varnish, or lacquer
coatings of high protective value.
Class IV – A coating consisting essentially of inorganic2 phosphates of zinc
or iron having a weight within the range 0.2 to 1.5 g/m of treated
surface. This class will normally be used where items are to be deformed
during further fabrication after the application of paint, varnish, or
lacquer.

NOTE: Dimensional changes resulting from phosphating treatments are

normally within a maximum increase of 8 µm/surface, depending on the
particular process selected and a strict adherence to the process
manufacturer’s operating instructions. Deviation from the specified
operating conditions of the phosphating solution can result in excessive
attack of the item with possible decrease in dimensions and uneven coatings
of inferior properties.
The dimensions of the finished item shall be those of the item after
phosphating and before the application of any supplementary finish. Where
phosphating is used to give anti-wear properties to sliding surfaces the
coating is consolidated during the running-in period, and consequently no
machining allowance should normally be made for phosphating.

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1 Scope
This Standard specifies requirements for the processing of iron and steel
(excluding corrosion-resisting steels) to produce coatings consisting
essentially of inorganic phosphates, which are intended to be used in
conjunction with supplementary finishes for the protection of the basis
metal against corrosion (and in certain cases to give, additionally, anti-
wear properties to sliding surfaces).
2 WARNING
This Standard calls for the use of substances and/or procedures that may be
injurious to health if adequate precautions are not taken. It refers only
to technical suitability and in no way absolves either the designer, the
producer, the supplier or the user from statutory and all other legal
obligations relating to health and safety at any stage of manufacture or
use.
3 Related Documents
3.1 The following documents and publications are referred to in this
Standard:
BS 427 Method for Vickers Hardness Test and for Verification of
Vickers Hardness Testing Machines
BS 970: Part 1 General Inspection and Testing Procedures and Specific
Requirements for Carbon, Carbon Manganese, Alloy and
Stainless Steels
BS 970: Part 3 Bright Bars for General Engineering Purposes
BS 3900: Part F4 Resistance to Continuous Salt Spray
BS 5466: Part 9 Saline Droplets Corrosion Test (SD Test)
Def Stan 03-2 Cleaning and Preparation of Metal Surfaces
Def Stan 03-4 The Pre-Treatment and Protection of Steel Items of
Specified Maximum Tensile Strength Exceeding 1450 MPa
Def Stan 03-7 Painting of Metal and Wood
Def Stan 03-29 Protection of Metallic Springs Against Corrosion
Def Stan 68-10 Corrosion Preventive Compound: Water Displacing.
NATO Code No: C–634, Joint Service Designation: PX-24
Def Stan 80-7 Paint, Priming, Red Oxide/Zinc Oxide, Air-Drying
Def Stan 80-25 Paint Finishing Ammunition Stoving. Paint Priming
Ammunition Stoving. Scheme A: System of Primer and
Finish. Scheme B: One Coat Finish.
Def Stan 80-27 Paint Finishing Ammunition: Paint Priming Ammunition.
Scheme A: System of Primer and Finish. Scheme B: One Coat
Finish.
Def Stan 80-34 Corrosion Preventive Compound: Oil Film Type, Joint
Service Designation: PX-4
Def Stan 80-44 Lacquer, Shellac, Type QX
Def Stan 80-56 Paint, Finishing, Epoxide, Stoving, Black for Small Arms.
Def Stan 80-92 Lacquer, Phenol-Formaldehyde, Stoving, Type QX, Grades
22%, 30%, 39%
Def Stan 91-40 Corrosion Preventive Oil, Aircraft Engine. Piston,
Metallic. NATO Code No: C-615, Joint-Service Designation:
PX-27

3.2 Reference in this Standard to any related document means in any

invitation to tender or contract the edition and all amendments current at
the date of such tender or contract unless a specific edition is indicated.

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3.3 The above series of documents are obtainable from the addresses shown
below:

DOCUMENT SOURCE

British Standards (BS) British Standards Institution

Sales Department
389 Chiswick High Road
LONDON W4 4AL

Defence Standards (Def Stan) Directorate of Standardization

Ministry of Defence
Kentigern House
65 Brown Street
GLASGOW G2 8EX

4 Definitions
For the purpose of this Standard the following definitions shall apply:
4.1 Process Control Schedule. The document which specifies/defines:
(a) The sequence of manufacturing operations and processes.
(b) The control parameters and their tolerances for each individual
process within the total sequence.

4.2 Significant surface. That area of the item, covered or to be covered

by the coating, and for which the coating is essential for serviceability
and/or appearance.
4.3 Unaccelerated process. An unaccelerated process is one in which the
processing solution is of the plain metal phosphate/phosphoric acid type
and no accelerating agents are employed.
4.4 Accelerated process. An accelerated process is one where the
processing solution is of the metal phosphate/phosphoric acid type
containing additions such as oxidizing agents, eg nitroguanidine, nitrate,
nitrite, or chlorate, which accelerate the coating formation.
4.5 Pointage. Pointage is a measure of the total acidity of a phosphating
solution. It is the number of millilitres (ml) of 0.1M sodium hydroxide
solution required to neutralize 10 ml of the phosphating solution to pH 10
using phenolphthalein as an indicator.
4.6 Free acid. The free acid of a phosphating solution is the number of
millilitres (ml) of 0.1M sodium hydroxide solution required to neutralize
10 ml of the phosphating solution to pH 4 using methyl orange or an
equivalent indicator system.
4.7 Sealing. Sealing is the application of a supplementary finish to the
phosphate surface immediately after phosphating, washing, and drying, to
form a complete protective or lubrication scheme.

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4.8 Supplementary finish. A supplementary finish is a coating material,

usually of an organic nature, eg oil, grease, lacquer, varnish, paint or
dry lubricant.
4.9 Tensile strength of steels
4.9.1 Throughout this Standard the tensile strength figures refer to
specified maximum tensile strength. Steels shall be categorized according
to specified maximum tensile strength in accordance with the table below.
Where the steel specification specifies only the minimum tensile strength,
the equivalent maximum tensile strength category shall be determined from
the following table:
Table A
Tensile Strength of Steels

SPECIFIED MINIMUM SPECIFIED MAXIMUM

TENSILE STRENGTH TENSILE STRENGTH
MPa MPa

Up to 1000 Up to 1100
Over 1000 to 1400 Over 1100 to 1450
Over 1400 to 1800 Over 1450 to 1800
Over 1800 Over 1800

4.9.2 Tensile strength/hardness relationship. If no maximum or minimum

tensile strength is specified for the steel hardness values of 310 HV,
340 HV, 435 HV, 450 HV and 545 HV (as measured in accordance with BS 427)
shall be regarded as equivalent to 1000, 1100, 1400, 1450 and 1800 MPa
respectively. Steels which have been wholly or partly surfaced hardened
shall be considered as being in the category appropriate to the hardness of
the surface hardened layer.
5 Information to be Supplied to the Processor
The following information shall be given on the drawing, contract or order:
(a) The number of this Defence Standard.

(b) The specification and metallurgical condition of the basis metal.

(c) The significant surface. This may be indicated on the drawing or by a
marked sample.
(d) The requirements for stress relieving of high strength steels,
(see clause 8).
(e) The class of phosphate coating required and the type of supplementary
finish required (eg oil, grease, paint, etc). These shall be designated as
for example: Phosphate Def Stan 03-11 Class II/Stoving Paint Def Stan
80-25 Scheme B.
(f) For creviced items, the phosphate process and/or nature of accelerator
employed.

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5 (Continued)

(g) For high strength steels, details of any special process requirements.
6 Process Control
6.1 A Process Control Schedule suitable of achieving the requirements of
this Standard shall be prepared by the processing contractor(s) prior to
the commencement of production.
6.2 Details of the coating process, including all preparatory treatments
and post coating treatments, processing, significant surface, tests and all
other processes and treatments shall be included in the Process Control
Schedule.
6.3 All stages in the complete Schedule shall follow each other without
delay.

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Section Two. Process Requirements

7 General
All items to be coated shall be prepared and treated in accordance with Def
Stan 03-2 or Def Stan 03-4 as appropriate. Care shall be taken at all
stages to prevent contamination of the surfaces being treated, eg by
touching with bare hands, and condensation of moisture after final drying.
8 Heat Treatment
If required, steel items shall be stressed relieved prior to phosphating in
accordance with Def Stan 03-2 or Def Stan 03-4 as appropriate.
9 Surface Preparation
All surfaces shall be free from grease, oil, oxide, scale, rust, paint or
other foreign matter. All items shall be degreased prior to the
commencement of a cleaning sequence, which shall be in accordance with Def
Stan 03-2 or Def Stan 03-4 as appropriate, to produce a chemically clean
surface. Items with folds, seams, or crevices shall receive special
attention to ensure removal of oil, grease, or other foreign matter. The
method of removal shall be chosen with due regard to its effect on the
properties of the item and the formation of high quality phosphate
coatings. After alkali or acid cleaning, the items shall be washed in cold
or hot water to remove all residues of cleaning materials that would
otherwise affect the quality of the coating or the efficacy of the
phosphating solution. Both acid and strong alkali treatments can result in
the formation of coarse crystalline phosphate coatings of poor quality.
Post cleaning conditioning treatments to prevent such coarse coatings may
be used.
10 Phosphate Treatment

10.1 Only processes capable of meeting the requirements of this Standard

shall be used. The process used shall be applied in accordance with the
agreed operating instructions for the process and in such a manner that
coating formation is complete, ie by proper attention to time of
phosphating, solution temperature and composition, and avoidance of gas
pockets where air or hydrogen from the treatment may become entrapped.
10.2 Normally plant should be constructed of steel and care should be
taken to avoid the use of unsuitable materials in plant construction,
eg copper or brass heating coils, which will contaminate the phosphating
solution and adversely affect the quality of the phosphate coating.
10.3 Processing of creviced items. Items with folds, seams, or crevices
shall receive special attention to ensure removal of oil or grease before
phosphating. Care shall also be given to the removal of treatment chemical
from such places, especially when an accelerated phosphating process has
been used (see clause 21).
10.4 Processing of composite items. Composite items made up of ferrous
and non-ferrous items shall normally have their ferrous items phosphated
before assembly. Exceptions can be allowed in cases of composite items
containing zinc base material or copper base material (the copper base
material should not normally constitute more than about 10 per cent of the
total surface) provided that the joint is unlikely to be penetrated by the
phosphating solution.
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 DEF STAN 03-11/3

10.5 Processing of high strength steels. Items made from steels with a
specified maximum tensile strength greater than 1100 MPa shall normally be
phosphated by a process of the accelerated (but copper free) type. Such
items shall be free from applied stress during processing and until
subsequent baking treatment has been completed. In the special case of
close coiled springs, these shall be slightly extended during treatment to
permit complete coverage and adequate washing. The amount of the extension
shall be the minimum required to achieve this and the constraint should be
removed immediately after post treatment washing and drying. Further
guidance on the treatment of springs is given in Def Stan 03-29. Further
advice on precautions to be taken to ensure satisfactory phosphate
treatment of high strength alloy steels is given in annex B.
11 Washing. To remove residues of the treatment solution, in particular
items with folds, seams or crevices (especially when an accelerated
phosphating process has been used), items shall be washed as follows (see
clause 21):
11.1 After treatment by an unaccelerated process, items shall be washed in
flowing cold water, then in either hot water (65°C minimum) or the hot
dilute ‘chromic’ solution (65°C minimum) described in 11.3.
11.2 After treatment by an accelerated process, items shall be washed
thoroughly, first in flowing cold water and then in hot water at a minimum
temperature of 75°C and finally washed in the hot dilute ‘chromic’ solution
described in 11.3. The accumulation of treatment chemicals in the rinse
waters shall be avoided by maintaining a sufficient flow of cold water and
by periodic renewal of hot water. The acidity of the hot water shall never
be allowed to exceed that corresponding to 0.75 ml of 0.1M sodium hydroxide
solution when tested by the method described in annex A or by a suitably
calibrated pH meter.
11.3 The ‘chromic’ wash solution (see NOTE) shall normally consist of not
more than 50 g nor less than 15 g of chromic acid, or of alkali metal
chromate or alkali metal dichromate, or of a mixture containing
approximately equal parts of chromic and phosphoric acids, per 100 litres
of water. A higher concentration than the maximum quoted in the previous
sentence shall not be used on surfaces which will be in contact with, or in
proximity to, explosives or propellants. In other cases higher
concentrations of chromic acid, chromate or dichromate may be used up to a
maximum of 500 g per 100 litres of water where such concentrations will
give overall beneficial results and where the effect of local enrichment or
drainage will not be detrimental under paint systems.
NOTE: The repeated handling with bare hands of items that have been given a
‘chromic’ wash may constitute a health hazard (chrome sensitivity
dermatitis).
11.4 The wash waters, hot or cold, used for unaccelerated and accelerated
processes shall not contain chloride, calculated as chloride ion, in excess
of 0.5 g/l when determined by the method described in annex A.
12 Staining
Staining black by water soluble dye, where required, shall be applied at
this stage. Staining by spirit dye compositions, where required, shall be
applied after drying.

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DEF STAN 03-11/3

13 Drying
Items shall be dried thoroughly after washing (preferably forced dried),
special attention being paid to items with pockets or crevices and also to
temperature limitations in clause 14.
14 Heat Treatment Relief of Hydrogen Embrittlement
14.1 Immediately after phosphating, washing and drying, and before
application of the supplementary finish, items made from steel of specified
maximum tensile strength within the range of 1100 to 1450 MPa (or of
equivalent surface hardness) shall be baked at 130 to 230°C for not less
than one hour. Items which have been surface hardened, eg by carburizing,
the temperature shall be restricted to a maximum of 140°C. For items with
soldered joints the temperature shall be restricted to a maximum of 130°C.
A temperature restriction may also apply to some springs.
14.2 Items made from steel of specified maximum tensile strength exceeding
1450 MPa are subject to the requirements of Def Stan 03-4.
14.3 Where stoving paint is applied and stoved immediately after
phosphating and the stoving schedule meets the requirements of 14.1
and 14.2 for de-embrittlement, as appropriate, no further baking treatment
is required.
14.4 De-embrittlement treatment at the higher temperatures may cause
slight colour changes and dehydration of phosphate coatings with consequent
lowering of corrosion resistance (particularly that of zinc phosphate
coatings).
15 Sealing
15.1 Immediately after washing, drying, and the baking treatment where
applied, the phosphate coating shall be sealed by the application of a
supplementary finish (but see 15.3). The type of finish required (eg oil,
grease, paint, etc) and, in the case of paint, varnish, or lacquer, the
weight or thickness of the coating, shall be as stipulated on the drawing,
contract or order. The finish shall normally be to Service standard.
Where no supplementary finish is stipulated, the treatment shall be
completed with a temporary protective, eg Corrosion Preventive Compound
PX-4 (Def Stan 80-34).
15.2 Where the items are required to be finished by paint, varnish, or
lacquer, and an interval between the phosphating and the first stage of the
supplementary finishing treatment is unavoidable the phosphated items shall
be kept under conditions which preclude contamination or condensation of
moisture on the surface.
15.3 When heavily pigmented primers are applied to a Class I or Class II
phosphate coating, complete impregnation may not be achieved, leading to a
serious lack of adhesion, particularly under dynamic conditions. When such
phosphate films are to be painted consideration should be given to using a
low viscosity impregnating coat of clear lacquer compatible with the normal
paint system (eg high bake epoxy lacquer at low viscosity), followed by the
normal paint system.
15.4 Further guidance on painting is given in Def Stan 03-7.

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Section Three. Inspection and Test

16 Inspection
All coated items shall be subject to visual inspection and representative
samples as specified below are to be subsequently tested.
17 Selection of Test Samples
17.1 Intermittent processing. Select two items. One shall be left
unsealed and tested as specified in clause 20 and the other shall be sealed
with the specified supplementary finish and tested as specified in
clause 21. These tests shall be carried out weekly.
17.2 Continuous processing. Select four items. TWO items shall be taken
within 30 minutes of the start and two taken within 30 minutes of the
finish of each production run or shift. One item of each pair shall be
left unsealed and tested as specified in clause 20 and the other shall be
sealed with the specified supplementary finish and tested as specified in
clause 22. When the Process Control Schedule requires the test specified
in clause 21 to be carried out, an additional phosphate item shall be
provided. This item shall be sealed with the specified supplementary
finish (see annex D).
Where the items are of a number, size or shape which make it impracticable
to carry out the tests specified in clause 20 or clause 22, test plates
(see annex E), of similar condition to and treated together with the actual
items being phosphated may be used. In the case of steels, a test plate of
the same composition and metallurgical condition shall be used.
17.3 If any of the items fail the tests the process shall be suspended
until the reason for failure has been established and further tests have
given satisfactory results. Items from the batch that failed and from
subsequent batches will have to be considered for re-treatment (see
clause 23).
18 Visual Inspection
18.1 The phosphate coatings should be uniform and matt in appearance and
there should be no untreated areas. However, phosphate coatings showing
minor variations in colour or surface texture, due to previous surface
treatments, heat treatments, or degrees of cold-work, shall be acceptable
provided they meet all other requirements of this Standard.
18.2 The coating shall be free from such residues of the phosphating
solution as may initiate deterioration of the supplementary finish or
premature corrosion.
18.3 Any superficial powdery deposit on the surface shall be removed,
eg by light brushing, but the method of removal shall not cause damage to,
or contamination of, the main coating.
19 Test for the Presence of a Coating
Where there is any doubt as to the presence of a satisfactory coating one
or more of the following tests shall be carefully applied:

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DEF STAN 03-11/3

19.1 Rub the treated surface with steel wool (grade 000). Untreated steel
shows a bright burnished appearance.
19.2 Scrape the surface once with a blunt knife. Coated surfaces show a
whitish streak.
19.3 Scrape a small area with a sharp knife. Coated surfaces yield a
light grey powder.
NOTE: Items which undergo and comply with these tests may be given the
appropriate finishing treatment and submitted with the remaining items of
the batch. Test methods 19.2 and 19.3 may not give very marked indications
of the presence of a Class III or Class IV coating.
20 Coating Weight
The coating weight, determined as described in annex C, shall meet the
following requirements:
Table B

Coating Weight

CLASS COATING
2
WEIGHT
g/m

min max

I 7.5 -

II 4.5 -
III 1.5 4.5

IV 0.2 1.5

21 Freedom from Corrosive Residues

The phosphated and sealed items shall be subjected to the test described in
annex D to confirm the efficiency of the washing procedure used. No rust
or other defect of the finish, eg blistering or flaking of paint coatings,
shall be visible at the end of the test.
22 Resistance to Salt Spray
After phosphating and application of the supplementary finish, the samples
shall be subjected to the salt droplet test described in annex E for tests
on actual items, but in the case of painted items a period of seven days
drying time shall be allowed for air-drying paint and four days for a
stoving paint. Twenty four hours shall be allowed before testing samples
sealed with oil or grease. Preliminary damage by scratching as described
in annex E shall be inflicted on painted, varnished, or lacquered items
before the test. After a test period, examples of which are given below,
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22 (Contd)
no rust shall be visible on the surface, but slight rusting at sharp edges
shall not be a cause for rejection. Where scratches have been inflicted,
no rust shall be visible beyond 5 mm and no blistering, lifting or flaking
beyond 1.3 mm from the original boundaries of the scratches.
Table C
Examples of Supplementry Finishes for Resistance to Salt Spray

ITEM SUPPLEMENTARY FINISH PERIOD

NO. (see NOTE) OF TEST
(days)

1 Corrosion preventive oil: PX-27 (Def Stan 91-40) 1

2 Corrosion preventive compound: PX-4 (Def Stan 80-34) 1

3 11% Lacquer, shellac, type QX (Def Stan 80-44) 1

4 Air drying paint, one coat (Def Stan 80-27 3
Scheme B)
5 Stoving lacquer (Def Stan 80-92) 6
6 Stoving paint, one coat (Def Stan 80-25
Scheme B
or Def Stan 80-56) 6

NOTE : This does not apply to Class III and Class IV coatings except
when a supplementary finish of stoved lacquer or stoved paint is used.
Where a two coat or multi coat paint system is to be used, the test
shall be conducted after the application of the first (priming) coat,
eg Def Stan 80-7, for a period of three days. The test periods given
apply when the finishes have been applied to normal standards of film
thickness appropriate to the supplementary finish in question. If an
item fails to pass the test by reason of general rusting, the fault may
lie with the application of the finish, eg too thin a film.

23 Re-Treatment of Items Rejected on Inspection

23.1 All supplementary finishes applied shall first be removed by a
suitable means, eg treatment by organic solvent, alkaline degreasant, etc
or abrasive cleaning. (See Def Stan 03-2 Methods A, B and D).
23.2 Phosphate coatings shall be removed by either grit blasting or
treatment in an acid solution, inhibited to prevent unacceptable attack on
the basis metal. Immediately after removing the defective phosphate
coating, the items should be re-phosphated in accordance with clause 10.

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NOTE 1: Suitable inhibited acid solutions for removing phosphate coatings

are given in annex C. The 10 per cent chromic acid solution may be used on
steels with a specified maximum tensile strength greater than 1100 MPa.
After removing the phosphate coatings, the items shall be thoroughly washed
to remove acid solution residues before re-phosphating.

NOTE 2: Where it is not possible to re-phosphate immediately after removal

of the defective phosphate coating, grit blasted items shall be dipped in
oil containing a corrosion inhibitor, eg material complying with Def
Stan 80-34. Items treated in inhibited acid shall be washed, dried and
similarly treated, or washed and dipped in a water displacing protective
fluid, eg material complying with Def Stan 68-10. Appropriate cleaning
operations (see clause 9) shall be carried out before re-phosphating.
NOTE 3: On certain items acid treatments before phosphating can impair the
quality of phosphate coatings although certain proprietary solutions
applied after acid treatment and before phosphating can have an
ameliorative effect. In order to obtain acceptable results it may be
necessary, in certain cases, to resort to mechanical methods, eg grit
blasting, to remove defective coatings before re-phosphating.

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 DEF STAN 03-11/3
ANNEX A

Determination of Rinse Water Contamination

A.1 Test for Carry Over of Treatment Solution
(a) Solutions required:
Sodium hydroxide: 0.1M sodium hydroxide solution.
Phenolphthalein indicator: Dissolve 0.5 g of phenolphthalein in 50 ml of
ethanol and dilute to 100 ml with distilled water.
(b) Procedure. Stir the contents of the rinse bath; withdraw about 100 ml
of the solution and cool to room temperature. Measure 50 ml of the cooled
solution into a 300 ml conical flask or other suitable glass container, add
a few drops of phenolphthalein indicator and titrate with the 0.1M sodium
hydroxide solution until a permanent faint pink colouration is obtained.
The titration value shall not exceed 0.75 ml.
A.2 Test for Chloride in Rinse Water
The following test is designed to determine when the rinse water contains a
chloride content in excess of 0.5 g/l:
(a) Solutions required:
Standard chloride: Solution containing 0.5 g/l of chloride ion. Dissolve
0.825 g sodium chloride in distilled water and dilute to 1 litre.
Acid silver nitrate solution: 1% m/v silver nitrate in 20% v/v nitric
acid. Dissolve 10 g of silver nitrate in a little distilled water, add
200 ml of nitric acid (specific gravity = d = 1.42) and dilute to 1 litre.
(b) Apparatus
Two 100 ml tubes.
One 5 ml measuring cylinder.
Two glass rods approximately 200 mm long and 5 mm diameter for stirring the
solutions.
(c) Procedure
(i) Mark the two 100 ml tubes ‘S’ and ‘T’ respectively, in any convenient
way.
(ii) To the tube marked ‘S’ add 5 ml of the standard chloride solution and
dilute to the 100 ml mark with water.
(iii) To the tube marked ‘T’ add 5 ml of the rinse water (see NOTE) and
dilute to the 100 ml mark with water.
NOTE : If the rinse water contains suspended matter it shall be filtered
through a Whatman No. 1 paper (or equivalent) before using it for the test.

A-1
DEF STAN 03-11/3
ANNEX A (Concluded)

A.2 (Contd)
(iv) To each tube add 5 ml of the silver nitrate solution. Stir the
contents of each tube with the glass rods, and set aside for one minute.
(v) Compare the turbidities of the two solutions. If the solution in tube
‘T’ is more turbid than that in tube ‘S’ then the rinse has a chloride
content greater than 0.5 g/l.

A-2
 DEF STAN 03-11/3
ANNEX B

Phosphating of High Strength Steels

B.1 Removal of rust and heat treatment scale by mechanical methods is

preferred (eg abrasive blasting). The use of acid solutions to remove rust
and heat treatment scale before phosphate treatment may be the cause of the
formation of unacceptable coarse crystalline phosphate coatings which may
allow light rusting to occur during subsequent rinsing and drying
operations. The quality of the phosphate coating may be improved by
brushing the surface of the metal under running water before phosphating,
to remove non–adherent residues insoluble in the acid solution.
B.2 In the case of certain low alloy steels, eg BS 970: Part 1, 897M39
(chromium-molybdenum-vanadium) and copper-silicon-molybdenum-vanadium
steels, the best phosphate coatings are obtained using accelerated
solutions. Considerable difficulties have been met in obtaining acceptable
phosphate coatings on the former type of steel particularly in the forged
form and it may be necessary to consider an alternative method of
protection.
B.3 The free acid concentration of the phosphate solution can markedly
affect the quality of the phosphate coating of alloy steels, eg BS 970:
Part 3, 826M31 (nickel-chromium-molybdenum) and maraging (nickel-cobalt-
molybdenum-titanium) type steels. It is recommended that the pointage to
the free acid ratio be maintained at not less than 6 to 1 to obtain
acceptable coatings and prevent unacceptable attack and/or pitting of the
steel during the phosphate treatment. The free acid level of the phosphate
process solution, which tends to increase when the bath is maintained at
the operating temperature but is not used, may be reduced by the treatment
of clean steel scrap, steel wool, or finely divided iron powder. Addition
of iron powder to the phosphate process solution may result in a vigorous
reaction. The iron powder should be added in small quantities and the
reaction allowed to subside after each addition before further iron powder
is added.

B-1
Blank Page
 DEF STAN 03-11/3
ANNEX C

Determination of Phosphate Coating Weight

NOTE: The coating weight shall be determined on an item after treatment by
phosphating, washing, and drying and before any heat treatment and sealing.
C.1 Normal Method
(a) Stripping solution. The following stripping solution may be used:
Dissolve 100 g of chromium trioxide in distilled water, dilute to 1 litre
and use at 90 to 95°C.
(b) Procedure. A convenient
2
surface area for the determination of coating
weight is about 100 cm . Weigh the item and immerse it in an unused sample
of the solution and allow it to remain in the solution until the coating
has dissolved (a period of five minutes is normally sufficient). Remove
the item from the solution, wash for 30 seconds in running water and wipe
off any non-adherent matter with a wet swab of cotton wool. Dry thoroughly
and re–weigh.
2 W
(c) Calculation. The weight of phosphate coating (g/m ) = A
Where W = loss in weight of the item in grams and

A = surface area in square metres.

C.2 Alternative Method
Where the phosphate item is too large to permit it being treated as in C.1
above, the following method , suitable for approximate practical purposes,
may be used:
(a) Stripping solution. Inhibited sulphuric acid: Dissolve 0.05 g of
di-o-tolylthiourea in 100 ml of sulphuric acid (d = 1.84).
(b) Procedure
(i) Dissolve the phosphate coating from a known area of the item. The
solution may be conveniently restricted to a known area by containing it in
an open ended glass or polythene tube stuck on to the unsealed phosphate
surface by cellulose varnish or other suitable adhesive (a convenient size
tube is one of approximately 40 mm diameter and approximately 40 mm in
length).
(ii) Determine the phosphate content of the solution used to dissolve the
phosphate coating. Any well recognized and reliable method for estimation
of phosphate may be used.
(iii) Calculation
3-
2.2 x amount of PO4 (g)
2
Coating weight (g/m ) = 2
Area stripped (m )

C-1
DEF STAN 03-11/3
ANNEX C (Concluded)

C.2 (Contd)
Using a tube 40 mm internal diameter, as described above, this formula
reduces to:
2 3-
Coating weight (g/m ) = 1751 x PO4 (g).

C-2
 DEF STAN 03-11/3
ANNEX D

Determination of the Freedom from Corrosive Residues

Suspend the item for seven days at a temperature of 15 to 25°c in a closed
vessel in which the atmosphere is kept humid by a layer of water in the
bottom of the vessel. At the end of this period, remove the item and
inspect it immediately for signs of rust or blistering of the paint film.

D-1
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 DEF STAN 03-11/3
ANNEX E

Salt Droplet Test

E.1 Test Specimens
E.1.l Where it is not possible to carry out the test on the actual item
(see 17.2), then test panels of the same material shall be used.
E.1.2 The test panels shall measure 150 mm x 100 mm (see Fig. 1). Two
holes 5 mm diameter and lightly countersunk on each side shall be drilled
at 6 mm from each edge near adjacent corners at the ends of a 100 mm side,
to enable the specimens to be suspended vertically during the test. All
cut edges and corners shall be lightly rounded off and smoothed.

Fig E.1 Test Panel

E.2 Test Procedure

E.2.1 The items or panels (see Fig. 1) shall be suspended vertically, by
means of hooks of glass or other non–corrodible insulators passing through
the holes in two corners, over large dishes partly filled with water. The
distance between the surface of the water and the lower edge of the items
or panels shall be 50-75 mm and the items or panels shall be one behind the
other and all face the same way. They shall be a convenient distance (not
more than 25 mm) apart to prevent touching when being moved and a dummy
item or panel shall be placed at each end of each row.
E-1
DEF STAN 03-11/3
ANNEX E (Continued)

E.2 (Contd)
E.2.2 Once daily, for five days a week, all the items or panels, including
the dummies, shall be removed temporarily from their position on the rack
and sprayed individually on both sides with the salt solution, using a hand
operated atomizer. The aim shall be to cover the surface with discrete
droplets, by giving a number of puffs with the nozzle at a suitable
distance (150-300 mm) from the specimens, the spray being directed, in
turn, at different parts of the surface. The spraying shall not be so
heavy that the droplets coalesce; in order to avoid this it may prove
necessary on occasions, where the surface is still wet from the previous
spraying, to refrain from applying the full weight of spray specified
below. It is essential to keep the items or panels covered with droplets.
Immediately after spraying, the items or panels shall be returned to their
positions on the rack and the whole collection shall be covered with a box-
like cover of sheet metal or other suitable material, to prevent the drying
of the droplets.
Any cover shall be suitably protected on the inside to prevent
contamination of the item or panel.
NOTE: The spray may be absorbed by non-glossy paint films; if so it may be
impossible to check that the desired distribution of droplets has been
obtained. The intensity of spraying required is shown in BS 5466: Part 9,
Fig. 2. This difficulty can be overcome by spraying dummy items or panels
of a material, (on which the droplets can be seen) in such a way as to
produce the standard distribution of droplets and then spraying the test
items or panels in exactly the same way. Steel or glass coated with a hard
glossy finish is suitable for this purpose.

E.2.3 The intensity of spraying can be checked by weighing the solution

deposited on both sides of a blank 150 mm x 100 mm freshly degreased bare
steel panel. The weight should lie between 0.5 and 1.0 g.
The temperature throughout the test shall be between 5°C and 20°C and the
test assembly shall be protected against external sources of heat tending
to produce local variations in temperature.
The spray solution shall be a synthetic sea water, in accordance with
BS 3900: Part F4.

E-2
 DEF STAN 03-11/3
ANNEX E (Continued)

E.2 (Contd)
E.2.4 Any atomizing nozzle capable of producing fine droplets (not a mist)
may be used for the test. The whole apparatus including the container
shall be made of non–metallic material, eg glass or ebonite.
E.2.5 There shall be two scratches, each 50 mm long, parallel and at a
distance of 50 mm apart (see Fig. 1), unless the size or shape of the
article does not permit this, in which case alternative arrangements shall
be permissible. In all cases, the scratch shall penetrate the paint film
to the substrate. The article shall be placed for test in such a way that
the scratches run vertically, thus eliminating any tendency for rust stain
to spread laterally from the scratches under the action of gravity.
No test shall commence within 24 hours of the completion of the coating
process and, if the items or panels are scratched before test, a further
interval of 24 hours shall elapse between the infliction of the scratches
and the first spraying.
E.3 Loss in Weight of Control Specimens
E.3.1 At the end of the agreed test period, the loss in weight of the
control items or panels shall be determined after de-rusting: The average
loss in weight shall be not less than the values given below:
Table C
Loss in Weight of Control Specimens

TEST DURATION AVERAGE LOSS IN WEIGHT

(DAYS) PER 150 mm x 100 mm PANEL
(GRAMMES)

5 1.0
7 1.4

14 2.4

21 3.3

28 4.1

E.3.2 The items or panels shall be de-rusted by means of Clarke’s

solution, which consists of 20 g of antimonious oxide and 50 g of stannous
chloride dissolved in 1 litre of hydrochloric acid (d = 1.16). The
solution shall be used cold and the items or panels kept moving in it until
de-rusting is complete. The items or panels shall then be washed in
running water, dried and weighed. The figure to be recorded is the
difference between the weight of the freshly degreased items or panels and
the corresponding weight after de-rusting.

E-3
EF STAN 03-11/3
ANNEX E (Concluded)

E.3 (Continued)
It is essential that the items or panels be kept moving in the solution so
as to ensure rapid reduction by the reagent of ferric chloride produced by
solution of the rust; otherwise attack on the steel itself may occur.
E.4 Inspection
E.4.1 At the end of the agreed test period the items or panels shall be
rinsed in cold water, visually inspected, and allowed to dry at room
temperature. Immediately the items or panels are dry a final inspection
shall be made.
E.4.2 The same procedure shall be followed if failure is suspected at an
earlier stage and if inspection confirms failure the items or panels
concerned may be removed from test.

E-4
 DEF STAN 03-11/2
ANNEX F

Approximate Conversion of Metric Units to Imperial Equivalents

SI Imperial Imperial SI Context Used

2 2
1 MPa 145 lbf/in 1 lbf/in 0.006895 MPa Tensile Strength
2 2
1 MPa 0.0209 lbf/ft 1 lbf/ft 47.88 MPa Tensile Strength
2 2 2 2
1 kgf/m 0.205 lbf/ft 1 lbf/ft 4.88 kgf/m Tensile Strength
2 3
1 g/ml 0.036 lbf/ft 1 lb/ft 27.679 g/ml Density

1 g/l 0.160 oz/gal 1 oz/gal 6.236 g/l Concentration

1 µm 0.000039 in 1 thou 25.4 µm Thickness

(mil in US)
2 2 2 2
1 A/m 0.0929 A/ft 1 A/ft 0.00107 A/m Current Density
2 2 2 2
1 A/dm 10 A/ft 1 A/ft 0.1 A/dm Current Density

lg 0.0353 oz 1 oz 28.349 g Weight

1 kg 2.204 lb 1 lb 0.454 kg Weight

1 ml 0.035 fl oz 1 fl oz 28.413 ml Volume

1l 0.220 gal 1 gal 4.546 l Volume

F-1
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DEF STAN 03-11/3

C Crown Copyright 1995

Published by and obtainable from: This Standard may be fully reproduced
Ministry of Defence except for sale purposes. The
Directorate of Standardization following conditions must be observed:
Kentigern House 1 The Royal Coat of Arms and the
65 Brown Street publishing imprint are to be
GLASGOW G2 8EX omitted.
2 The following statement is to be
Tel No: 041-224-2531/2532 inserted on the cover:
Fax No: 041-224-2503 ‘Crown Copyright. Reprinted by
(name of organization) with the
permission of Her Majesty’s
Stationery Office.’
Requests for commercial reproduction
should be addressed to MOD Stan 1,
Kentigern House, 65 Brown Street,
GLASGOW G2 8EX

The following Defence Standard file reference relates to the work on this
Standard - D/D Stan/313/11/1 (Stan 5c).

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Defence Standards are revised when necessary by the issue either of
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matter may be investigated and appropriate action taken.

90/50061