Def Stan 03 20 Issue2

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Ministry of Defence

Defence Standard

03-20/Issue 2 31 MARCH 1994

ELECTRO-DEPOSITION OF ZINC

This Defence Standard


supersedes
Def Stan 03-20/1 dated
8 December 1980
DEF STAN 03-20/2

AMENDMENTS ISSUED SINCE PUBLICATION

AMD NO DATE OF TEXT AFFECTED SIGNATURE &


ISSUE DATE

Revision Note

Historical Record

DTD 903D dated March 1966


Def Stan 03-20/1 dated 8 December 1980
DEF STAN 03-20/2

ELECTRO-DEPOSITION OF ZINC
PREFACE

This Defence Standard supersedes


Def Stan 03-20/1
dated 8 December 1980

i This Defence Standard specifies the requirements for the Electro-


Deposition of Zinc.
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 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
applications 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 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 for 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.

1
DEF STAN 03-20/2

CONTENTS PAGE

Preface 1

Section One. General


1 Scope 3
2 WARNING 3
3 Related Documents 3
4 Definitions 4
5 Information to be Supplied to the Processor 5
6 Process Control 5

Section Two. Process Requirements

7 General 6
8 Heat Treatment 6
9 Surface Preparation 6
10 Zinc Plating 6
11 Washing 7
12 Passivation 8
13 Heat Treatment Relief of Hydrogen Embrittlement 8

Section Three. Inspection and Test


14 Inspection 9
15 Selection of Test Samples 9
16 Visual Inspection 9
17 Adhesion 9
18 Thickness of Coating 9
19 Freedom from Mercury 10
20 Retreatment of Items Rejected on Inspection 10

Table A Thickness Requirements 7


Table B Heat Treatment Requirements 8

Annex A Method for the Determination of Mercury A-1


Annex B Adhesion Tests B-1
Annex C Method for the Determination of Average Thickness C-1

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DEF STAN 03-20/2

ELECTRO-DEPOSITION OF ZINC

Section One. General


1 Scope
This Standard specifies the requirements for the electro-deposition of zinc
on non-corrosion resisting steel items for protection against corrosion,
and on copper-based alloy items and corrosion resisting steel items for the
reduction of contact corrosion of less noble metallic materials.
Zinc coatings shall not be used on items which are liable to be subjected
to temperatures exceeding 350°C.
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 heath and safety at any stage of manufacture or
use.
3 Related Documents
3.1 The documents and publications referred to in this Standard are listed
below:
BS 427 Methods for Vickers Hardness Test and for Verification
of Hardness Testing Machines
BS 2656 Specification for Zinc Anodes, Zinc Oxide and Zinc Salts
for Electroplating
BS 5411 Methods of Test for Metallic and Related Coatings
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 03-14 Electro-Deposition of Chromium for Engineering Purposes
Def Stan 03-21 Mechanical Methods for the Inducement of Compressive
Surface Residual Stresses
Def Stan 03-33 Chromate Passivation of Cadmium and Zinc Surfaces
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.
3.3 The above series of documents are obtainable from the addresses shown
below:

3
DEF STAN 03-20/2

3.3 (Contd)

DOCUMENT SOURCE

British Standards (BS) British Standards Institute


Sales Department
Linford Wood
MILTON KEYNES MK14 6LE

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 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 Tensile strength of steels
4.3.1 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:

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

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DEF STAN 03-20/2

4.3.2 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 surface hardened
shall be considered as being in the category appropriate to the hardness of
the surface layer.
5 Information to be Supplied to the Processor
The following 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 process to be used.
(e) The details of any pre and post-deposition heat treatment.
(f) The thickness of the coating required.

(g) The details and thickness of any necessary undercoat to be applied.


(h) The details of any finishing treatment required.
(i) The details of any special requirements (eg masking).
6 Process Control
6.1 The Process Control Schedule shall be agreed by the responsible
Technical or Supervising Authority named in the contract or order prior to
the commencement of production. The agreed Schedule shall not be altered
without prior written agreement of the responsible Technical or Supervising
Authority.

6.2 Details of the coating process, including all preparatory treatments


and post coating treatments, processing, thickness of coating, significant
surfaces, test and all other processes and treatments shall be included in
the Process Control Schedule.
6.3 All stages in the complete schedule, unless otherwise agreed by the
responsible Technical or Supervising Authority, shall follow each other
without delay.

5
DEF STAN 03-20/2

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.
8 Heat Treatment
If required, steel items shall be stress relieved prior to the electro-
deposition of zinc in accordance with Def Stan 03-2 or Def Stan 03-4 as
appropriate.
9 Surface Preparation
All surfaces shall be free from solids such as soap, drawing compounds,
oil, grease, machine fluid, polishing compounds etc, discoloration, oxide
scale 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. Drying by means of chlorinated solvents is not permitted.
Any shot peening of the basis metal shall be carried out before the
application of the coating and shall be in accordance with Def Stan 03-21.
10 Zinc Plating
10.1 Electrolyte. Zinc may be electro-deposited from various electrolytes
each having limitations and advantages. Any process meeting the
requirements of this Standard may be used subject to the limitations of
Def Stan 03-4. The supplier or user of the materials employed for making
up and maintaining the electrolyte shall certify them as free from mercury
when tested by the method given in annex A or by any other method agreed by
the responsible Technical or Supervising Authority. Care shall be taken to
avoid accidental contamination of the electrolyte with mercury.
10.2 Anodes. Zinc anodes shall conform to the requirements of BS 2656 and
in addition shall be certified by the supplier as free from mercury when
tested by the method described in annex A or by any other method agreed by
the responsible Technical or Supervising Authority.
10.3 Materials other than steel. Items made from materials other than
steel may, at the discretion of the responsible Technical or Supervising
Authority, be plated with a suitable undercoat to an agreed thickness
before zinc plating.

10.4 Locally chromium plated items. Where items are to have local areas
hard chromium plated, that operation and any subsequent heat treatment in
the range 400 to 480°C (see Def Stan 03-14) shall be carried out prior to
zinc plating.
10.5 Thickness requirements. The electro-deposited coating shall be
smooth and adherent, and shall conform to the minimum thickness
requirements detailed in table A.

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DEF STAN 03-20/2

10.5 (Contd)
In certain cases, where it is necessary to conform to the tolerance
requirements of mating items or where interchangeability considerations
apply, it may be necessary to impose additional limitations on the
thickness of the coating. In such instances the requirement shall be
stated on the drawing, contract or order.
Table A
Thickness Requirements

LOCAL AVERAGE
APPLICATION THICKNESS THICKNESS
µm µm

1. Normal requirements. 10 min 14 min

2. Threaded items 3 mm to 20 mm dia 8-14 10 min


(see NOTE 2), screws, bolts and
nuts of nominal major thread
diameter.
Close tolerance items less than 4-7 6 min
3 mm dia.

3. Washers. 3-7 5 min

4. Rivets, taper pins, and split cotters. 5-10 8 min

NOTE 1: For barrel plated items average thickness is normally based on the
whole sample, but if used for vat plated items it is normally based on
individual items.
NOTE 2: The coating thickness requirements for threaded items are dictated
by dimensional tolerance limits. Such thicknesses will not necessarily
provide adequate protection against corrosion in all applications.
11 Washing

The electroplated items shall be washed in clean running water to remove


the electrolyte, then dried.

7
DEF STAN 03-20/2

12 Passivation
12.1 Items shall be chromate passivated to the requirements of Def Stan
03-33, unless otherwise specified.
12.2 Items shall be passivated immediately after plating and washing
unless requiring relief from hydrogen embrittlement in which case heat
treatment shall take place before passivation.
NOTE: Process control of passivation is required to prevent excessive
conversion of the zinc coating.
13 Heat Treatment Relief of Hydrogen Embrittlement
13.1 Plated steel items shall be heat treated in accordance with table B
as soon as practicable but within 4 hours of plating.
Table B
Heat Treatment Requirements

SPECIFIED MAXIMUM SPECIFIED MINIMUM


TENSILE STRENGTH TENSILE STRENGTH TEMPERATURE TIME (MINIMUM)
OF STEEL OF STEEL
MPa MPa °C hours

up to 1100 up to 1000 Not applicable

over 1100 to 1450 over 1000 to 1400 190 to 230 8

over 1450 over 1400 See Def Stan 03-4

13.2 Plated steel items having surface hardened areas eg carburising and
through-hardened or bearing steels which would suffer an unacceptable
reduction in hardness by treatment in accordance with table B shall be heat
treated at a lower temperature but not less than 130°C for a minimum of
6 hours.

8
DEF STAN 03-20/2

Section Three. Inspection and Test

14 Inspection
All plated items shall be subject to visual inspection and representative
samples as specified below are to be subsequently tested in the following
order for adhesion, thickness and freedom from mercury.
15 Selection of Test Samples
15.1 A sample comprising 1% of each vat or barrel load, but not less than
8 items or more than 48 shall be selected for tests, the number of items
selected to be such that significant weighing errors are avoided.
15.2 Where a continuous form of vat plating is in operation,
representative samples shall be selected at intervals of not more than
1 hour.
15.3 The sample shall be divided into equal parts, one part for thickness
tests and one part for adhesion tests.
15.4 In exceptional circumstances, eg the vat plating of a single large
item or the barrel plating of a small number of items, the sampling
procedure specified in 15.1, 15.2 and 15.3 may be modified. Coupon samples
plated together with the items may be used, due consideration being given
to their shape, size, material and if applicable, position in the vat. The
treatment of the coupon samples shall be representative of that applied to
the items being plated.
15.5 If any part of a sample fails a test, a further sample shall be
selected and the test repeated. If this sample fails, the vat or barrel
load represented by this test shall be rejected.

16 Visual Inspection
At the conclusion of all processing all items shall be inspected to ensure
that the coating is smooth, continuous, uniform in appearance, is free from
stains, burns, blisters, exfoliation, pits, nodules, cracks, porosity,
uncoated areas, excessive edge build up or other defects and show no
indication of improper use of equipment.
Items shall be clean and free from damage. Unavoidable contact marks may
be allowed with prior agreement of the responsible Technical or Supervising
Authority.
17 Adhesion
When tested in accordance with any of the methods described in annex B,
there shall be no indication of the deposit becoming blistered or otherwise
detached from the base metal.
18 Thickness of Coating
18.1 General. Local thickness tests shall be made except that, with prior
agreement of the responsible Technical or Supervising Authority, an average
thickness test may be substituted on items, such as small barrel plated
items, which are considered unsuitable for local thickness determination.

9
DEF STAN 03-20/2

18.2 Local thickness. The local thickness of the coating shall be


determined by one or more of the following methods.
(a) Micro-sectioning (BS 5411, Part 5)
(b) Coulometric (BS 5411, Part 4)
(c) Electromagnetic (BS 5411, Part 11) (ferrous substrates)
(d) Beta backscatter (BS 5411, Part 12)
(e) X-ray spectrometric (BS 5411, Part 8)
The referee method is the micro-section method (BS 5411, Part 5).
18.3 Average thickness. The average thickness of the zinc coating and
where applicable, the nickel undercoat, shall be determined by the weight
loss methods described in annex C.
For barrel plated items the average thickness shall be based on the whole
sample, but if used for vat plated items it shall be carried out on the
individual items comprising the sample.
19 Freedom from Mercury
Evidence of freedom from mercury in coatings shall be proven by periodic
testing in accordance with the method given in annex A or any other method
agreed by the responsible Technical or Supervising Authority.
20 Retreatment of Items Rejected on Inspection

If for any reason items are required to be stripped of their coating and
recoated the procedure shall be in accordance with a Process Control
Schedule agreed by the responsible Technical or Supervising Authority.
Steel items shall be subject to the requirements of Section Two,
immediately after stripping.

Steel items with specified maximum tensile strengths over 1450 MPa shall
not be reprocessed without the prior written agreement of the responsible
Technical or Supervising Authority.

10
ANNEX 03-20/2
ANNEX A

Method for the Detection of Mercury


A.1 Mercury in Salts
A.1.1 Make up as required, an alkaline stannous chloride solution by
dissolving 1.2 g of stannous chloride in 20 ml of water, disregarding the
precipitate formed by hydrolysis. Pour, whilst stirring, into 20 ml of 20%
sodium hydroxide solution and continue stirring until the precipitate is
dissolved.
A.1.2 Using the salts to be tested, dissolve in water 10 g of sodium
cyanide, 6 g of sodium hydroxide and 10 g of zinc cyanide in that order.
Filter and dilute to 100 ml in a suitable cylinder.
A.1.3 Alternatively, if zinc oxide is used to make up the bath instead of
zinc cyanide, dissolve 15 g of sodium cyanide and 6 g of zinc oxide, filter
and dilute.
A.1.4 Add 2 ml of the alkaline stannous chloride to the solution referred
to in A.1.2 or A.1.3 above and mix. A turbidity indicates the presence of
mercury and is visible if 0.0002 g or more is present.
A.2 Mercury in Electrolyte
Test 100 ml of solution with alkaline stannous chloride as described
in A.1.
A.3 Mercury in Anodes
Dissolve 5 g of the anode in 50 ml of nitric acid (d = 1.42). Dilute the
solution with about 50 ml of water, boil to remove oxides of nitrogen and
cool. Dilute the solution further to 100 ml in a suitable cylinder.
Immerse a 75 mm length of clean 1.6 mm dia. copper wire in the solution and
allow it to remain for 15 minutes. A deposit on the copper wire indicates
the presence of mercury and will be seen if 40 ppm or more is present in
the anode.
A.4 Mercury in Coating
Cut a piece of clean steel sheet 120 mm x 120 mm, which has been
electroplated to produce a zinc coating 5 µm thick, into pieces 40 mm
square and place the pieces in a 250 ml beaker. Pour 25 ml of hot
(60-80°C) nitric acid (d = 1.42) over the pieces, completely covering them,
and swirl the beaker until effervescence has ceased. Transfer the liquid
to another beaker, rinse the specimens with cold distilled water and add
the rinsings to the main solution. Boil the solution to remove oxides of
nitrogen, cool and dilute to 100 ml in a suitable cylinder and test as in
A.3. A deposit will be visible on the copper wire if the test solution
contains 0.0002 g or more of mercury.

A-1
Blank Page
DEF STAN 03-20/2
ANNEX B

Adhesion Tests
B.1 Burnishing Test
2
Rub an area of approximately 1 cm of the plated surface rapidly and firmly
with the end of a suitable smooth tool for about 15 seconds and visually
inspect. There shall be no indication of the deposit becoming detached
from the basis metal. The pressure applied should be sufficient to burnish
the coating at each stroke, but not so great as to cut the deposit.
B.2 Bend Test
The item under test shall be bent once through 180°, or until fracture,
over a mandrel having a radius equal to twice the thickness of the sample
(minimum radius 1.5 mm). On visual inspection there shall be no indication
of the deposit becoming detached from the basis metal.
B.3 Quenching Test
Heat the plated samples under test in an oven to a temperature of 185 ±
15°C and then quench in water at room temperature. On visual inspection
there shall be no indiction of the deposit becoming detached from the basis
metal.

B-1
Blank Page
DEF STAN 03-20/2
ANNEX C
Methods for the Determination of Average Thickness
C.1 Determination of Average Thickness of Zinc Coating
C.1.1 Clean the plated sample in a suitable solvent vapour, weigh and then
totally immerse in a solution prepared by dissolving 30 g of ammonium
nitrate in 100 ml of water. Stir the solution occasionally until the
plating is dissolved, 10 minutes being usually sufficient. Remove the
sample from the solution, wash, dry and reweigh.
3
Loss in mass (g) x 140 x 10
Zinc thickness (µm) = 2
Area of coating (mm )
alternatively:
C.1.2 Clean the plated sample in a suitable solvent vapour, weigh and then
totally immerse in a solution containing 2.5 g of antimony trichloride and
600 ml of hydrochloric acid (d = 1.16) per litre. Stir the solution
occasionally until the plating is dissolved, two minutes being usually
sufficient. Immediately effervescence has ceased, remove the sample from
the solution, wash, dry and reweigh.
3
Loss in mass (g) x 140 x 10
Zinc thickness (µm) = 2
Area of coating (mm )
NOTE: Antimony and its salts have a significant effect on hydrogen
embrittlement of steels.
C.2 Determination of Average Thickness of Nickel Undercoat on Copper-Base
Materials
After the thickness of the zinc coating has been estimated, immerse the
sample in a solution of 70% (v/v) sulphuric acid (d = 1.84) with a little
glycerine added. Treat anodically at 6 to 12 volts. Immediately solution
of the nickel is complete, remove sample, wash rapidly, dry and reweigh.
3
Loss in mass (g) x 113 x 10

Nickel thickness (µm) = 2


Area of coating (mm )

C-1
Blank Page
DEF STAN 03-20/2

o
c Crown Copyright 1994 This Standard may be fully reproduced
except for sale purposes. The
Published by and obtainable from: following conditions must be observed:
Ministry of Defence 1 The Royal Coat of Arms and the
Directorate of Standardization publishing imprint are to be
Kentigern House omitted.
65 Brown Street 2 The following statement is to be
GLASGOW G2 8EX inserted on the cover:
'Crown Copyright. Reprinted by
Tel No: 041-224-2531/2532 (name of organization) with the
Fax: 041-224-2503 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/313/03/04 (Stan 5c).

Contract Requirements

When Defence Standards are incorporated into contracts users are


responsible for their correct application and for complying with contract
requirements.

Revision of Defence Standards

Defence Standards are revised when necessary by the issue either of


amendments or of revised editions. It is important that users of Defence
Standards should ascertain that they are in possession of the latest
amendments or editions. Information on all Defence Standards is contained
in Def Stan 00-00 (Part 3) Section 4, Index of Standards for Defence
Procurement - Defence Standards Index published annually and supplemented
periodically by Standards in Defence News. Any person who, when making use
of a Defence Standard encounters an inaccuracy or ambiguity is requested to
notify the Directorate of Standardization without delay in order that the
matter may be investigated and appropriate action taken.

93/50009
DIRECTORATE OF STANDARDIZATION

MINISTRY OF DEFENCE
Stan Ops 5d, Level One,
Kentigern House, 65 Brown Street,
Glasgow, G2 8EX
Tel: 0141 224 2679
Fax: 0141 224 2503

Your reference: Def Stan 03-20/2

Our Reference: D/D Stan 313/03/04

Date: 21 November 1996

AMENDMENT NOTICE

Def Stan 03-20/Issue 2

ELECTRODEPOSITION OF ZINC

Amendment 1 (Revised Text)

This notice has been agreed by the authorities concerned with the use of
the above Standard.

1. Page 7, Table A

Delete: In toto

Insert: "New Table attached"

2. Make a note of this Amendment in the Amendment Record.

H McLERNON
for Directorate of Standardization
Table A

Thickness Requirements

MINIMUM MINIMUM
LOCAL AVERAGE
APPLICATION THICKNESS THICKNESS
(see Note 1)
µm µm

1. Normal requirements:

Steels (non-corrosion resisting) 10 14


Copper-base materials and 8 12
corrosion resisting steels

2. Threaded items not exceeding 20mm dia.


(see Notes 2 and 3), screws ,bolts and
nuts of nominal major thread diameter:

up to 3mm 4
Over 3mm up to 5mm 5
Over 5mm up to 13mm 6.5
Over 13mm up to 20mm 7.5

3. Washers 5

4. Rivets, taper pins and split cotters 8

NOTE 1: For barrel plated items average thickness is normally based on the whole sample, but if used
for vat plated items it is normally based on individual items.

NOTE 2: Thickness requirements for copper-base materials are inclusive of nickel undercoating.

NOTE 3: The coating thickness requirements for threaded items are dictated by dimensional tolerance
limits. The thickness specified will not necessarily provide adequate protection against corrosion in all
applications.

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