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DOWTY PROPELLERS STANDARD PRACTICES MANUAL

NDT 6DAP
ETCH INSPECTION OF STEEL COMPONENTS

1. General

A. This specification details the requirements to inspect the surfaces of fully heat treated non-stainless
steel parts for conditions which can be revealed by submitting the part to an acid etch procedure.

B. Conditions which can be revealed by the use of acid etch procedures described in this specification
are as follows:

(1) Re-tempered and re-hardened areas due to abusive grinding. This also applies to other
machining operations on ultra high strength steels.

(2) The effectiveness of any grinding, honing or lapping operations on nitrided or case hardened
parts. This includes the removal of ‘white layer’ on nitrided areas, and the unevenness and
break-through of case hardened or nitrided layers.

(3) Determination of the thickness of the hardened layer subsequent to machining operations which
section a nitrided or case hardened region.

(4) Resolution of the location and effectiveness of an induction hardened region.

(5) The general condition of ‘as heat treated’ surfaces on through hardened steels, when local
areas of decarburisation can be detected.

(6) Any abuse to the surface which affects the hardness locally, e.g. seizure of a machining steady,
local burns due to inefficient electrical contact during plating or magnetic particle flaw detection.

C. NDT 6DAP supersedes NDT 6 for all future Dowty Propellers contracts.
Where existing drawings/documents call up NDT 6, NDT 6DAP must be used in lieu.

2. Applicability

A. The requirement to acid etch will be stated on the drawing.

B. It is required to be carried out:

(1) On all through hardened non-stainless steels with a specified maximum tensile strength in
excess of 1450 Mpa (95 ton/in2).

(2) On all non-stainless steels which have been subjected to surface hardening treatments such as
carburise case hardening, nitriding and induction hardening, (treated regions only).

(3) High strength steels which are to be chromium plated with a specified maximum tensile strength
in excess of 1230 Mpa (80 ton/in2).

(4) When Dowty Propellers (DP) or any of its sub-contractors are etching parts for other main
contractors, then the procedure used must satisfy that customer’s specification requirements.
The exception is when such a main contractor has approved DP’s methods in lieu of its own.

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3. Associated Specifications

A. PS 5100 - Cadmium Plating

B. PS 5201 - Vapour Blasting

C. PS 5202 - Temporary Corrosion Protection of Parts

D. PS 5203 - Trichloroethylene Vapour Degreasing

E. PS 5900 - General Manufacturing Standards

F. PS 51000 - Use of Specifications in Manufacturing

G. PS 51004-4-1 - Machining Special Techniques for Ultra High Tensile Steels

H. NDT 10DAP - Approval of Personnel for Non-destructive Testing

I. BS M37 - British Standard Aerospace Series. Method for the Etch Inspection of
Metallic Materials and Components

J. SBAC - Technical Memorandum for ‘The Etch Inspection of Steel Surfaces for the
Detection of Grinding Abuse

K. II 26 - Calibration of Stop Watches & Mechanical Timers

4. Equipment & Materials

A. Select from the following according to the requirements of the ‘Method’ to be employed.

(1) Suitable sized acid resistant containers.

NOTE: Every container used during the acid etch process must be clearly identified with
the name of its contents.

(2) Cold water rinse tank fitted with an overflow and drain pipe. The tank must be fed continuously
with clean running water when in use, and should therefore be provided with suitable effluent
disposal facilities, such as a coke and lime filter to drain.

(3) De-watering oil tank, with grid or inclined bottom and drain shelf. As water will sink to the
bottom of the tank a drain tap is recommended.

(4) Nitric acid. Specific gravity 1.42.

(5) Hydrochloric acid. Specific gravity 1.16.

(6) Industrial methylated spirit (de-natured alcohol).

(7) Anti-smutting agent. Type JAR-3N, obtainable from:-

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Devonshire Consulting & Marketing Ltd.,

Unit 19 Ambron House Business Centre,
East Field Road,
Wellingborough,
Northants,
NN8 1QX Tel: 01933 270361 Fax: 01933 277736

(8) De-watering oil (PS 5202).

(9) Filtered air supply.

(10) Soft bristle scrubbing and bottle brushes.

(11) Protective gloves.

(12) Safety glasses or visor.

(13) Scotchbrite pads, type S, supplied by:-

3M United Kingdom PLC.

5. Etching Procedure

CAUTION: REPEATED ETCHING OF INDIVIDUAL COMPONENTS MUST BE AVOIDED.

CLEARANCE MUST BE OBTAINED FROM A SENIOR NDT TECHNICIAN OR THE
MATERIALS LABORATORY BEFORE ETCHING MORE THAN THREE TIMES.

A. Non-stainless steels currently used by DP can all be etched adequately to meet the requirements
given in para 1.B. using a nitric acid solution as the basic etchant. The variations to the basic
etchant are given in Part 6, ‘Etching Methods’ of this specification and related to the conditions of
steels on which they can be used.

WARNING: WEAR SAFETY GLASSES AND SUITABLE GLOVES.

B. The general etching procedure consists of certain primary operations, these can be sub-divided in
order to satisfy a particular method. The primary operations are as follows:-

(1) Pre-cleaning. The last cleaning operation is normally vapour de-greasing. Prior to this, heavy
films or other deposits must be removed by operations such as paraffin wash or vapour blast as
for MAT 102.

(2) Immersion in the nitric acid solution.

(3) Post etch neutralizing/cleaning.

(4) Protection from corrosion.

(5) Inspection.

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C. Where parts require de-embrittlement due to acid etch being performed, it will be called up as a
separate operation on the Manufacturing layout unless a later stress relief operation satisfies the
requirement. PS 5100, Section 9, times and temperatures under column heading ‘Stress Relief
Before Plating’ shall be used. For parts in steels over 1800 MPa the de-embrittlement operation
shall be carried out within 4 hours of etching, in which case this will satisfy the pre-plating stress
relief requirement.

D. Where the ‘as etched’ surface is detrimental and/or is required to be removed, the drawing will state:
‘AFTER ETCHING, REWORK SURFACES TO PS 51000’. The requirement should also be
called up as a separate operation on the Manufacturing Layout.

6. Etching Methods

A. This section details the etching methods, relating each to the materials to which they can be applied.
The detailed procedure for each method then follows. Refer to Part 8, Solution and Process
Controls for control requirements.

B. Method N1 - Nitric Acid in Methylated Spirit Etch with Hydrochloric Acid in Methylated Spirit Post
Etch & Cleaning.

(1) This method is for use on carburised and nitrided steels. It can also be used on the smaller
sized components in through hardened steels. De-embrittlement is required as specified in
para 5.C. This method should not be used on maraging steels (MAT 5102) or on plated parts.
Due to the fire hazard, solutions should rarely exceed 4,5 litres (1 gallon) in quantity.

(2) Procedure

WARNING: OBSERVE SAFETY PRECAUTIONS

(a) Vapour degrease (PS 5203) and allow to cool to room temperature.

(b) Immerse in methylated spirit and scrub clean.

(c) Immerse in 3% to 5% nitric acid/methylated spirit solution and gently agitate. Local
application by cotton wool swab is a permitted alternative. Time will depend on solution
strength, material and temperature, and normally range between 15 seconds and 120
seconds.

(d) Scrub in cold running water to remove smut.

(e) Immerse in methylated spirit.

(f) Immerse in 4% to 6% hydrochloric acid in methylated spirit and gently agitate for between
10 and 60 seconds.

(g) Scrub in cold running water to remove smut.

(h) Blow dry with filtered air supply.

(i) Immerse in de-watering oil (PS 5202) for 60 seconds and allow to drain.

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(j) Inspect (Refer to applicable Drawing for areas affected, and Part 7 for interpretation of
indications).

C. Method N2 - Nitric Acid and Anti-smutting Agent.

(1) This method is for use on all through hardened, maraging, nitrided and carburised steels. It is
also suitable for copper, bronze and chrome plated parts in these materials. De-embrittlement
control is not required due to the method eliminating the use of hydrochloric acid. The etch is
normally non-smutting.

(2) Procedure.

WARNING: OBSERVE SAFETY PRECAUTIONS

(a) Vapour blast to PS 5201 on maraging steel (MAT 5102). Ensure all parts are free of
heavily contaminated grease prior to para (b).

NOTE: First off etching will not require the vapour blast operation if carried out within
approximately 24 hours of grinding.

(b) Vapour degrease to PS 5203.

(c) Immerse in clean water to cool.

(d) Immerse in 3% nitric acid, 3 to 6% anti-smutting agent in water. Times will vary between 20
seconds and 180 seconds according to material surface condition and specification.

NOTE: A light to medium matt grey appearance on machined surfaces indicates

sufficient etching.

(e) Thoroughly rinse in clean water. A light smut may occur, on over-etched parts and on
some carburised surfaces, which can easily be removed by water/air spray gun or soft
brushing.

(f) Blow off excess water with filtered air supply. DO NOT attempt to completely dry.

(g) Immerse in de-watering oil to PS 5202.

(h) Inspect (See applicable Drawing for areas affected, and Part 7 for interpretation of
indications).

D. Method N3 - Nitric Acid in Methylated Spirit.

(1) This method is partly an alternative to Method N2 but only for use on small parts because of the
fire risk. It can be used for local application on large components by swabbing.

(2) The solution should be in a clean, comparatively little used condition, and should be discarded
as soon as a yellowish tinge appears, this improves the resultant reading as staining is less
likely to occur. EN19C should not be etched by this method. Where parts are copper plated,
this method is permissible for the shortest immersion time compatible with a readable result.

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(3) Procedure.

WARNING: OBSERVE SAFETY PRECAUTIONS

(a) Vapour blast to PS 5201 on maraging steel (MAT 5102).

NOTE: First off etching will not require the vapour blast operation if etched within
approximately 24 hours of grinding.

(b) Vapour de-grease to PS 5203 and cool to room temperature.

(c) Immerse in 3% to 5% nitric acid in methylated spirit solution. Time will depend on solution
strength, material and temperature, but will normally be between 15 seconds and 120
seconds.

(d) Scrub in cold water wash to remove smut.

(e) Immerse in methylated spirit for a few seconds.

(f) Immerse in de-watering oil (PS 5202) for 60 seconds and allow to drain.

(g) Inspect (See applicable Drawing for areas affected, and Part 7 for interpretation of
indications).

7. Inspection & Interpretation

A. Etched parts shall be inspected for surface imperfections appropriate to the material and/or for the
depth of case or nitrided layer when required by the drawing.

B. Whatever the part, areas which have not been machined or ground after heat treatment will normally
exhibit a darker shade of grey to black appearance to those which have. Light or silvery areas on
unmachined surfaces may indicate decarburisation on a through hardened part or local areas of
contamination. (Silicone based cutting fluids are one cause of such contamination).

C. Areas which have been ground, honed or lapped after heat treatment on nitrided parts should exhibit
a light matt grey colour compared to unmachined surfaces. Areas which show a light silvery white
appearance with darker boundaries compared to the uniform matt grey, are areas where the
operation has failed to remove the white (friable) layer. This indication can be confused with
grinding burn unless it is realised that it does not usually coincide with the ‘grinding wheel’ pattern of
a burn.

D. Light areas compared to the normal uniform matt grey appearance of nitrided or carburised parts
may indicate unduly thin case or nitrided layer. Dark zones, although uniform, may indicate general
lack of hardness. This should not be confused with the variations between the grey shades which
occur on unmachined areas, machined areas and ground areas. Misinterpretation can also result
due to staining, reference example in para 7.B. If doubt exists, the etch bloom should be removed
by vapour blast or grey Scotchbrite pad, and the part re-etched, either completely or locally as the
situation warrants.

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E. Grinding abuse can normally be identified by the fact that it shows as a regular pattern coincident
with the relative movement between the part and the grinding wheel, whether the surface be
carburised, nitrided or through hardened. Dark streaks or flecks against the uniform grey
background indicate local softening due to the operation causing local hot spots in the ‘temper
range’ of the material. When silvery white areas occur inside the local dark streaks or flecks, this is
due to the local heating reaching the ‘hardening range’ for the material. When the tempering
temperature for a material is 500 °C and above, it becomes difficult-to-impossible to discern any
darker region surrounding the silvery indication of a re-hardened area. Local large areas of burn
may be encountered on rare occasions. Examples are:-

Grinding wheel rotating on stationary part (safety device on machine failed). Difficult grinding
operation, when wheel has to reverse direction while still in contact. Seizure of a fixture steady - this
usually results in a circumferential burn. On ultra-high strength steels all the conditions of this
paragraph apply.

F. Small radii, the roots of gear teeth, and similar difficult regions should be inspected under
approximately X2 magnification.

G. Normally, temper or re-hardening burns on gear teeth or bearing tracks, or the presence of soft
spots, shall be cause for rejection. This also applies to through hardened steels in the ultra-high
tensile range (above 1800 Mpa). Re-hardening burn is always cause for rejection. On other areas,
or lower strength materials, some degree of softening may be permitted.

H. Inspection Disposal of Through Hardened Parts.

(1) The following procedure applies to all acid etch inspection stages:

(a) Re-hardening.

1 Where the etch indicates area of re-hardening the Reject Note is to state Re-hardening
- stress relieve 200 °C for 4 hours before any re-work.

(b) Temper Burning.

1 Quote ‘Temper Burn’ on the Reject Note and allow to proceed on normal re-work.

I. When there are indications on areas which have not been machined after heat treatment, or where
there are indications on machined areas which cannot be definitely interpreted by Inspection, the
matter is to be referred to the Company Metallurgist.

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8. Solution & Process Controls

A. Make-up of Solutions.

WARNING: ACID OR ALKALINE CONCENTRATES MUST NOT BE PLACED INTO THE

CONTAINER UNTIL AT LEAST 50% OF THE DILUTING AGENT IS PRESENT IN
THE CONTAINER. PROTECTIVE CLOTHING AND A FACE VISOR MUST BE
WORN DURING THE MAKE-UP OPERATION. CARE MUST BE TAKEN NOT TO
INHALE THE VAPOUR FROM THE CONCENTRATES. SHOULD A PERSON
INADVERTENTLY COME IN CONTACT WITH A CONCENTRATE, THE IMMEDIATE
ACTION IS TO WASH THE AREA WITH COPIOUS AMOUNTS OF CLEAN WATER,
THEN REPORT TO THE MEDICAL DEPARTMENT. IN THE DILUTED FORM,
CONTACT WITH THE EYES SHOULD STILL BE TREATED WITH CLEAN WATER
AND REPORTED.

(1) The initial make-up of a solution is to conform to the ratios given in Table II for the particular
method used.

B. Solution & Facilities Control.

(1) Where solutions are maintained for a period, checks of the solution strengths are to be made on
a monthly basis. Samples should be submitted to the laboratory for testing in accordance with
LAB 065: Free Acidity of Nitric Acid Etch Bath. The results are to be reported and held by NDT.

A satisfactory result = 25-35 grs / Ltr +/- 2 grs.

If the solution is under 25 the solution is weak and more acid should be added.

If the solution is over 35 the solution is strong and water should be added.

(2) When water based nitric solutions are used and the solutions maintained for long periods,
performance checks are to be carried out before use by processing a known ‘burnt’ test piece,
and the Control Sheet (ref. Para 10) must then be stamped by the Inspector.

(3) On small systems when solutions are to be changed daily, clear reference must be made on the
Control Sheet (ref. Para 10) to this effect. The change of solution or fresh mix must be further
supported by the immediate processing of a test piece, which again must be processed at the
start of each shift, and duly recorded.

(4) Inspect solutions before use for contamination and scum.

(5) All compressed air used for drying shall be adequately filtered at the point of use to remove oil,
water and solid particles. Filters shall be periodically inspected and properly maintained to
ensure satisfactory operation.

(6) When an acid etch system has not been in use, a clear statement to this effect must be made in
the relevant day/night block on the Control Sheet (ref. para 10).

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(7) White inspection lighting is to be a minimum level of 2000 Lux (200 ft candles) at the work top.
Monitoring of the lighting level is to be carried out monthly and recorded on the Control Sheet
(ref. Para 10).

(8) A timing device, which displays minutes and seconds, shall be available at the work station to
ensure compliance with the time limits laid down. The timer will be calibrated 6 monthly in
accordance with II 26, (or other acceptable procedure). Calibration intervals are specified in II
12A.

9. Acid Etch Application Summary

Table 1A
Material Category

NOTE: Strengths are maximum specified tensile stress.

Category Material Material Conditions Surface Conditions

1 Nitrided Steels Nitride Hardened Ground, Honed or Lapped
(Not Maraging)
Core Over 1450 MPa (95 tonf/in2) Machined Surfaces Not Nitrided
2 Carburising Steels Carburised and Hardened Ground
2
and EN19C Core Over 1450 MPa (95 tonf/in ) Machined Surfaces Not Carburised
3 Through Hardened Steels Over 1450 MPa (95 tonf/in2) Machined Surfaces
(Not Maraging)
Over 1100 MPa (70 tonf/in2) Ground Surfaces When Specified
4 Maraging Steels Hardened Machined Surfaces
Nitrided Hardened Ground, Honed or Lapped
2
Copper, Bronze or Over 1450 MPa (95 tonf/in ) Machined Steel Surfaces
Chrome Plated Parts
Over 1100 MPa (70 tonf/in2) Ground Surfaces if Specified

Table 1B
Frequency Rating

A 1st off of each batch/run

B 10% of each batch/run
C 100% on completion of all relevant operations
D 100% as produced

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Table 2
Solutions - Make Up and Control

Methods Solution Initial Make-Up Control Limits

N1 Nitric Acid 4% in Methylated Spirit 3% to 5% by volume, but
normally change each shift.
N3
N2 Nitric Acid 3% 2½ % to 3½% by volume
in water
Anti-smutting Agent 3 - 6% (Refer to NOTE)
N1 Hydrochloric Acid 5% in Methylated Spirit 4% to 6% by volume, but
normally change each shift

NOTE: It is not possible to measure quantities once in solution. Anti-smutting agent strength is not
critical but small additions should be made if smutting occurs within the normal etching times
and conditions.

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10 Acid Etch Control Sheet

DAYSHIFT

1 2 3 4 5 6 7

8 9 10 11 12 13 14

15 16 17 18 19 20 21

22 23 24 25 26 27 28

*29 *30 *31

NIGHTSHIFT

1 2 3 4 5 6 7

8 9 10 11 12 13 14

15 16 17 18 19 20 21

22 23 24 25 26 27 28

*29 *30 *31

Solution Details (See Table 2)

Nitric Acid/Meths./4% by volume
Hydrochloric Acid/Meths./5% by volume
Nitric 3%/JAR-3N 3% to 6%/Water by Volume
Fresh Mix Daily

Lights Mat Lab Timer DAILY CHECKS

Due: Process Burnt Test Piece
Scum & Contamination

MONTHLY CHECKS
White Lights 2000 Lux (200 ft candles)
Laboratory Checks

6 MONTHLY CHECK
Timers

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