BUREAU VERITAS

VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

Contractor’s Name : BUREAU VERITAS VIETNAM

Company’s Name : Nghi Son Refinery and Petrochemical LLC.

Plant Location : Nghi Son, Viet Nam

W/ Order No. :
Package No. : 5

Scope of Work : INSPECTION SERVICE FOR DCSM

Discipline : DCSM

NSRP DCSM PROJECT 2019

Discipline
Receiving Date
Reviewed By
Review Date
Review Result code
Document Review codes:
1- Rejected (Revise and resubmit), 2- Comments as Noted (Revise and
resubmit. Work may proceed subject to full compliance with comments),
3- Minor Comments (Acceptable, Works may proceed. Revise &
Resubmit as “Certified Final), 4- No comments (Works may Proceed)
Returned on
Next Submission Due
Date

THIS DOCUMENT IS CONTROLLED BY THE BUREAU VERITAS - VIETNAM AND MAY NOT BE AMENDED, REVISED OR ALTERED IN
ANY OTHER WAY WITHOUT THE CONSENT OF THAT COMPANY.

THE SIGNATURES BELOW AUTHORISE ALL PAGES OF THIS PROCEDURE FOR USE FROM THE DATE OF APPROVAL AS SHOWN.

Rev Date Description Prepared By Reviewed by Approved By

.
0 26/09/2019

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 BUREAU VERITAS
VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

Nguyen Gia Dinh Annamalai Natarajan Annamalai Natarajan

REVISION HISTORY

Rev. Date Issued Comments Prepared by Reviewed & Approved by

00 25.Sep.2019 First Issue. Nguyen Gia Dinh Annamalai Natarajan

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 BUREAU VERITAS
VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

INDEX

Section Description Page

1.0 Scope 04

2.0 Objective 04

3.0 Apparatus & Materials 05

4.0 Specimen Preparation Technique 05

5.0 Working Procedure – Examination of Replica by LM 08

6.0 Working Procedure – Examination of Replica by SEM 08

7.0 Results / Conclusions 10

8.0 Safety 10

9.0 Reference 10

Attachment 1 Report Format 11

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 BUREAU VERITAS
VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

INSITU METALLOGRAPHIC REPLICA TESTING

1.0 SCOPE:

1.1 To carry out Macro Etching, In-situ Metallographic Examination with replication of
microstructure and Investigation on material characterization with estimation of remnant
life for all applicable equipment’s, accessories, components constructed by metallic
materials in refinery plant at Vietnam.

2.0 OBJECTIVE:

2.1 To detect degradation that causes micro structural changes on the examined surface
and assess its fitness for further service.

3.0 APPARATUS & MATERIALS:

3.1 EQUIPMENT TO BE USED AT SITE:

3.1.1 Portable Metallurgical Microscope.

3.1.2 Portable Hand Grinding Machine

3.1.3 Portable Polishing Unit with Diamond Lapping Compound

3.1.4 Electrolytic Polisher cum Etching Unit

3.1.5 Etching Chemicals and Reagents as per table.

3.1.6 Emery grit sizes- Self-adhesive 30mm dia. SIC 120, 220, 300, 500 grits

3.1.7 Replica Kit : Polishing papers, sylvet cloth, polishing media, thermo setting or
thermo plastics, Cellulose acetate replica foils of 0.030 micron size.

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NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

3.2 EQUIPMENTS TO BE USED AT LABORATORY:

3.2.1 Laboratory Optical Microscope- 50X to 1000X Magnification: Dewinter /

Mitutoyo Make.

3.2.2 Sputter Coater, 2-20 nano meter Thickness to be Coat: Leica/Jeol make.

3.2.3 Scanning Electron Microscope – 1000X-10000X Magnification: JEOL Make.

4.0 SPECIMEN PREPARATION TECHNIQUE:

4.1 GRINDING:

4.1.1 Flatten the specimen with hand grinder to minimum depth to get surface free
from pin holes/ scaling/ pitting/surface corrosions and care to be taken not to
go too deep nor more than 1.0 mm from surface.

4.1.2 Grind the surface with emery papers (80- Grit to 1000 Grit Paper) should be
done in a particular direction to that of proceeding paper.

4.1.3 Once the Grinding steps are completed, the area is ready for Polishing.

4.2 Polishing:

4.2.1 Wash the sample thoroughly and finally polish by the Portable Polisher Using
Lavigated Aluminium oxide Suspension or Magnisium oxide Suspension (i.e
6-micron diamond compound followed by 1-micron diamond compound
polish).

4.2.2 Once the polishing steps are completed, the area is ready for Etching.

4.3 Etching:

4.3.1 To etch the reagents in the mirror finished surface of the test required
locations as per table-1.

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NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

Table-1: Etching Reagents for Micro Examination (For Ferrous & Non-Ferrous Metals)

S.NO ETCHING REAGENT METHOD REMARKS

Nital:
Swabbing for few seconds to a Carbon Steel, Low and Medium
1. Nitric acid (HNO3)= 1-5 ml
minute. alloy steel.
Ethyl Alcohol = 95 -100 ml

2. Picral: Picric acid 4 gm alcohol 100 ml do do

Hydraulic acid –5 ml For revealing the austenite grain

3. Picric acid --1 gm size in quenched and tempered
do
Alcohol --100 ml steels.

Ferric chloride –5 gm For Hydrochloric microstructure of

4. Acid - 50 ml austenitic nickel & steel
do
Water -100 ml

Nitric acid –10 ml For microstructure of austenitic

5. do
Alcohol --90-95 ml nickel steel.

For microstructure of Iron Chromium

Nitric acid --10 ml
Warm specimen in water base alloys, high speed steels,
6. Hydrochloric acid –20-30 ml
before etching austenitic manganese steels, nickel
Glycerin 1-5ml
chromium alloys.

Hydrochloric acid 30 ml For Stainless Steel alloys other

7. Apply Swabbing
Acetic acid 20 ml alloys high in Nickel or Cobalt.

Picric acid –10

For depth of case and structure of
8. Parts (4%)
do Nitro alloy.
Nitric acid –1 part (4%)
Copper Sulphate –4 gm
Hydrochloric acid-20 ml For total depth of
9. Swabbing
Water --20 ml Nitrided case.
(Marbles Reagent)

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NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

4.4 Replication:

4.4.1 A small piece of cellulose acetate, 3 to 5mm thick and approximately three
times the size of the area to be replicated, is held by tweezers and softened
on one side only.

4.4.2 Apply acetone with an eyedropper, allow setting for approximately 30

seconds, and then shake to remove excess acetone.

4.4.3 The soften side is then pressed firmly against the area with the eraser end of
a pencil or tip of the fingers and helped several seconds.

4.4.4 Care must be taken that the acetate is not allowed to slip or a smudged
replica will be obtained.

4.4.5 Let the replica remain in this position until it hardens, usually 10 to 15 minutes,
depending upon the size of the replica.

4.4.6 Once it has hardened it can be stripped with tweezers.

4.4.7 At this point the stripped replica should be put into a separate container
(usually a small Plastic box, or taped to a glass slide with double-sided tape.

4.4.8 Several Replicas should be made of each area and should be labeled
appropriately.

4.5 Labeling of Replica Slits ( Identification Marks):

4.5.1 The Replicated spot marked as XXXX-R-YY, XX is the short name of Client
and YY is the replica number, It will stars from 01,02..,etc and the same will
marked in the replica slit as an Identification of Replica and also the same will
revert all documents and reports for traceability.

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 BUREAU VERITAS
VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

5.0 WORKING PROCEDURE – EXAMINATION OF REPLICA BY LM:

5.1 Examination of replica carried out with the Metallurgical Microscope at 50X, 100 X, 200X,
400X/500X/1000X and photographs can be taken and also semi quantitative evaluations
can be made.

5.2 Examine the replicated Specimen in Metallurgical Microscope under 100 X & Higher
Magnification for the following.

5.2.1 Microstructure, Grain Size

5.2.2 Conditions of Metal,

5.2.3 Decarburization if any

5.2.4 Internal Granular Cracks if any, Any other Micro Defects.

5.3 The Microphotographs can be taken for any of the above features, if desired on
Metallurgical Microscope.

6.0 WORKING PROCEDURE – EXAMINATION OF REPLICA BY SEM:

6.1 Sample Preparation for SEM-Sputter Coating:

6.1.1 Sputter coating for SEM is the process of applying an ultra-thin coating of
electrically-conducting metal – such as gold (Au), gold/palladium (Au/Pd),
platinum (Pt), silver (Ag), chromium (Cr) or iridium (Ir) onto a non-conducting
or poorly conducting specimen.

6.1.2 Sputter coating prevents charging of the specimen, which would otherwise
occur because of the accumulation of static electric fields.

6.1.3 It also increases the amount of secondary electrons that can be detected from

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VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

the surface of the specimen in the SEM and therefore increases the signal to
noise ratio.

6.1.4 Sputtered films for SEM typically have a thickness range of 2–20 nm.

6.1.5 Benefits for SEM samples sputtered with metal:

6.1.5.1 Reduced microscope beam damage

6.1.5.2 Increased thermal conduction

6.1.5.3 Reduced sample charging (increased conduction)

6.1.5.4 Improved secondary electron emission

6.1.5.5 Reduced beam penetration with improved edge resolution

6.1.5.6 Protects beam sensitive specimens

6.2 SEM Analysis:

6.2.1 After prepared Sample of replica carried out with the Scanning Electron
Microscope at 1000X, 2000X/5000X/10000X and photographs can be taken
and also semi quantitative evaluations can be made.

6.2.2 Examine the replicated Specimen in SEM under 1000 X & Higher
Magnification for the following.

6.2.2.1 Surface Morphology

6.2.2.2 Microstructure,

6.2.2.3 Grain Boundary Degradations if any

6.2.2.4 Phase Transitions (if any)

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VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

6.2.2.5 Conditions of material

6.2.2.6 Observations of Gamma, Delta Ferrites If construction of Material

in Steel

6.2.2.7 Voids, Internal Granular Cracks( if any)

6.2.2.8 Any other Micro Defects.

6.2.2.9 The Microphotographs can be taken for any of the above features, if
desired on Metallurgical Microscope.

7.0 RESULTS / CONCLUSION:

7.1 The examined microstructure of the replica by LM and SEM with photographs and
quantitative evaluations can be made and the same report to the Client.

8.0 SAFETY:

8.1 Before using or mixing any chemicals, all product labels and pertinent Material Safety
Data Sheets (MSDS) should be read and understood concerning all of the hazards and
safety precautions to be observed.

8.2 All chemicals are potentially dangerous; person using any etchants should be thoroughly
familiar with all of the chemicals involved and the proper procedure for handling by use
proper protective equipment (Glass, Gloves, apron etc.)

9.0 REFERENCE:

9.1 ASM Hand Book Vol.9: Metallography and Microstructures.

9.2 ASM Hand Book Vol. 17: Nondestructive evaluation and quality control.

9.3 ASTM E1351, Standard Practice for production and Evaluation of Field Metallographic
Replicas.

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NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

9.4 ASTM E 407, Standard Practice for Micro etching Metals and Alloys.

9.5 ASTM E-03 Standard guide for Preparation of Metallographic Specimen.

9.6 ASTM E 114, Standard Test Methods for Determining Average Grain Size.

9.7 API RP 571, Damage mechanisms affecting fixating equipment in the refining industry.

9.8 API RP 573, Inspection of Fired Boilers and Heaters.

9.9 API RP 576, Inspection of Pressure relieving devices.

9.10 API RP 578, Material Verification Program

9.11 API RP 579, Fitness for Services.

9.12 API RP 580, Risk Based Inspection.

9.13 VGB-TW507e, Guideline for Creep Damage classifications for high pressure and high
temperature service components.

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 BUREAU VERITAS
VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

ATTACHMENT 1
REPORT FORMAT

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VIETNAM
NSRP DOCUMENT No.:
DCSM PROJECT 2019 INSITU METALLOGRAPHIC D-P5-BV-PD-014

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