insitu metallograhy report

1.0 INTRODUCTION

NFL Nangal isthe first key industry set up by Govt. Of INDIA with coming up of Bhakhra Dam &

surplus power

fertilizer plant at Nangal, which went to production in 1961.

Ammonium Nitrate (25% Nitrogen) and heavy water.

Plant based on fuel oil gasification which added Urea

1990. Electrolysis plant was replaced with Front End Plant(NMP

Naphtha production of hydrogen and reducing the electrical power con

2.0 IN-SITU METALLOGRAPHY

In

any degradation or abnormality present in the equipment due to the operational conditions.

Pressure and temperature plays an

plain carbon, medium carbon and high alloy steels used in different process plant application.

Principally, addition of alloying elements increases ability to withstand severe process demands

by gener

out on operating plants for various reasons like, condition assessment, life assessment to avoid

failure and for safe and reliable operation. Due to critical assessment

components, microstructural evaluation of the component has become powerful tool.

The technique of in situ metallography involves location s&polishing / electrolytic polishing, electrolytic etching or chemical etching, replication and microstructural observation. The kit of inlight

CUSTOMER

NATURE OF TEST

TEST REFERENCE

DATE OF TESTING

SAMPLE DRAWN

First floor, Thangavel NagarContact: +91

INTRODUCTION


surplus power available from the project at the time. It was derived by Govt. Of India to set a






SITU METALLOGRAPHY

In-Situ Metallographic testing is carried out to determine the conditions with respect to





by generating proper metallurgical conditions in an alloy. Various NDT Inspections are carried




The technique of in situ metallography involves location spolishing / electrolytic polishing, electrolytic etching or chemical etching, replication and

microstructural observation. The kit of in

CUSTOMER

NATURE OF TEST

EST REFERENCE

DATE OF TESTING

SAMPLE DRAWN

Metz Lab Private Limited

First floor, Thangavel Nagar+91-8190810222 | Mail:


available from the project at the time. It was derived by Govt. Of India to set a






SITU METALLOGRAPHY –

Situ Metallographic testing is carried out to determine the conditions with respect to





ating proper metallurgical conditions in an alloy. Various NDT Inspections are carried





microstructural observation. The kit of in

NATIONAL FERTILIZERS LIMITED,NAYA NANGAL

INSITUASM Vol.9,17 & ASTM E 1351,ASTM E 407.09 To 11

By Customer @


First floor, Thangavel Nagar, Walajabad Main Road,8190810222 | Mail: - [email protected]

Test Report








METHOD



Pressure and temperature plays an important role in degradation mechanism for alloys like








microstructural observation. The kit of in-

NATIONAL FERTILIZERS LIMITED,NAYA NANGAL

INSITU-METALLOGRAPHYASM Vol.9,17 & ASTM E 1351,ASTM E 407. 09 To 11-May

By Customer @


Walajabad Main Road,[email protected]

Test Report




Ammonium Nitrate (25% Nitrogen) and heavy water. Subsequently In 1978 went an A






important role in degradation mechanism for alloys like








-situ metallography comprises of portable grinder,

NATIONAL FERTILIZERS LIMITED,NAYA NANGAL,PUNJAB-

METALLOGRAPHYASM Vol.9,17 & ASTM E 1351,

May-16

By Customer @ NFL Nangal


Walajabad Main Road, [email protected] | website:

Test Report



fertilizer plant at Nangal, which went to production in 1961. The plant at that time produce

Subsequently In 1978 went an A

Plant based on fuel oil gasification which added Urea (46% Nitrogen) to its main product in












The technique of in situ metallography involves location selection, mechanical grinding polishing / electrolytic polishing, electrolytic etching or chemical etching, replication and

situ metallography comprises of portable grinder,

NATIONAL FERTILIZERS LIMITED, -140126

METALLOGRAPHY ASM Vol.9,17 & ASTM E 1351, API-571

NFL Nangal


Mannivakkam – 600 048| website:- www.metzlab.org



The plant at that time produce

Subsequently In 1978 went an A

(46% Nitrogen) to its main product in

1990. Electrolysis plant was replaced with Front End Plant(NMP-I) based on reforming of

Naphtha production of hydrogen and reducing the electrical power consumption.








failure and for safe and reliable operation. Due to critical assessment requirement of plant


election, mechanical grinding polishing / electrolytic polishing, electrolytic etching or chemical etching, replication and


REPORT No: MT /SBI /001


600 048 www.metzlab.org

Date : 28/05




Subsequently In 1978 went an Ammonia


I) based on reforming of

sumption.








requirement of plant





1 of 27

5/2016




mmonia


I) based on reforming of








requirement of plant




grinder with variable speed controlle

consumables. The consumables can be listed as self

size, self-

electrolytes and replica films

3.0 DAMAGE MECHANISMS THAT ARE DETECTED THROUGH MICROSTRUCTURESTUDIES

Damage mechanisms that are common to a variety of industries including refining and

petrochemical,

The principle deterioration mechanisms that could be detected by using in situ

metallographic

creep, hydrogen attack, carburization, grain boundary oxidization and em

microstructure etc. Aspects of each will be considered in turn. Depending upon the alloys used

and microstructure conditions with expertise on interpretations skills many other mechanisms

and damages can be predicted.

3.

involves time dependent deformation and high temperature creep cracking, develops at

grain boundaries in

include boiler super

petrochemical furnace and react

temperatures, with local over

strains and wall thinning. At

higher stress level. The fracture is eventually intergranule in nature. Classification of

creep damage in the components exposed to creep range has been made using the

largely qualitative approach based

observed by in situ metallography. The three stages of creep and associated

microstructure degradations are represented in the sketch given below. Basic guidelines

for evaluation of creep damage and provide

given in Table. In situ metallography used in conjunction with semi quantitative tools




-adhesive velvet cloth, solvents, water bottles, diamond paste, and suspended alumina,

rolytes and replica films

DAMAGE MECHANISMS THAT ARE DETECTED THROUGH MICROSTRUCTURESTUDIES


petrochemical, pulp and paper, and fossil utility are covered in this Sectio


metallographic techniques are the microstructural degradation like Spheroidization of pearlite,





3.1. CREEP DAMAGE:

Creep is


grain boundaries in

include boiler super















adhesive velvet cloth, solvents, water bottles, diamond paste, and suspended alumina,

rolytes and replica films



pulp and paper, and fossil utility are covered in this Sectio


techniques are the microstructural degradation like Spheroidization of pearlite,





CREEP DAMAGE:

Creep is one of the most serious high temperature damage mechanisms. It


grain boundaries in engineering components that fail over an extended time. These

include boiler super-heate













grinder with variable speed controller, electrolytic etcher/polisher, microscope and variety of











one of the most serious high temperature damage mechanisms. It


engineering components that fail over an extended time. These

heater and other components operating at high temperature,

petrochemical furnace and reactor vessel components and gas turbine blades. At higher

temperatures, with local overheating, deformation may be localized with large plastic

strains and wall thinning. At somewhat lower temperatures and under correspondingly










r, electrolytic etcher/polisher, microscope and variety of

consumables. The consumables can be listed as self-adhesive polishing papers of different grit













and other components operating at high temperature,

vessel components and gas turbine blades. At higher

eating, deformation may be localized with large plastic

somewhat lower temperatures and under correspondingly



on distribution of creep voids and micro cracks



for evaluation of creep damage and provide judgment on the inspection intervals are





adhesive polishing papers of different grit






















judgment on the inspection intervals are




REPORT No: MT /






pulp and paper, and fossil utility are covered in this Section.






















REPORT No: MT / SBI /001








creep, hydrogen attack, carburization, grain boundary oxidization and em-brittlement of

















2 of 27

SBI /001







lement of

















like hardness measurements indicating loss of tensile strength would permit remaining

life assessment

at this juncture is that

by displaying spheroidzation of carbides but with little void formation.



life assessment

at this juncture is that





life assessment studies on components undergoing creep damage. A point worth noting

at this juncture is that the chrome Molly steels are liable to fail by creep in a short time





studies on components undergoing creep damage. A point worth noting

the chrome Molly steels are liable to fail by creep in a short time
















REPORT No: MT /











3 of 27

SBI /001




3.2

penetrate inside. Thus, the thickening of grain boundaries in carbon steels can be seen

with etching

3.

temperature to

steel can be found out

3.

decreases the

examination.

3.

instance, sigma

temperature or cycled

loss of ductility an

embrittlement phenomenon when

400

checks are employed after exten

developing. Cracks can initiate from the brittle

resistance to bending. This can be detected by

are compared with the normal microstructures

of degradations.


3.2 HIGH TEMPERATURE OXIDATION:

Under highly oxidizing atmosphere grain boundary oxidization takes place that


with etching response

3.3. DECARBURISATION:

The carbon in the steel can react with oxygen and in the atmosphere at high

temperature to

steel can be found out

3.4. GRAIN COARSENING:

Grain coarsening takes place with prolonged high temperature exposure which

decreases the

examination.

3.5. EMBRITTLEMENT AND CARBURIZATION

Embrittlement

instance, sigma

temperature or cycled

loss of ductility an


400oC. If the temperature conditions are





of degradations.



HIGH TEMPERATURE OXIDATION:



response during

DECARBURISATION:


temperature to get decarburization of the surface. The loss of carbon in the surface of

steel can be found out from microstructure examinations

GRAIN COARSENING:


decreases the strength of the steel. This can be easily noticed by microstructure

examination.

EMBRITTLEMENT AND CARBURIZATION

Embrittlement from precipitations arise in a number of different ways for

instance, sigma phase formation in austenitic stainless steels maintained at high

temperature or cycled through the critical temperature range of 565 to 989

loss of ductility and embrit


C. If the temperature conditions are





of degradations.






during insitu metallography.

DECARBURISATION:


get decarburization of the surface. The loss of carbon in the surface of

from microstructure examinations

GRAIN COARSENING:


strength of the steel. This can be easily noticed by microstructure


from precipitations arise in a number of different ways for

phase formation in austenitic stainless steels maintained at high

through the critical temperature range of 565 to 989

mbrittlement. Ferritic stainless steels may be subjected to

embrittlement phenomenon when held at or cooled over the temperature range 550 to

C. If the temperature conditions are










metallography.



from microstructure examinations







tlement. Ferritic stainless steels may be subjected to

held at or cooled over the temperature range 550 to

C. If the temperature conditions are likely to lead to such effects, metallographic

checks are employed after extended exposure



are compared with the normal microstructures on comparison basis to





metallography.



from microstructure examinations.








likely to lead to such effects, metallographic

ded exposure prior to an unexpected rupture

developing. Cracks can initiate from the brittle carburized layer, which has little

resistance to bending. This can be detected by metallography.

on comparison basis to



REPORT No: MT /













prior to an unexpected rupture

carburized layer, which has little

metallography. Normally the damages

on comparison basis to












through the critical temperature range of 565 to 989 oC causes






Normally the damages

judge the extent

4 of 27

SBI /001









C causes






Normally the damages

judge the extent

4.0 PROCEDURE FOR INSITU METALLOGRAPHY EXAMINATIONS

4.1.

Naya Nangal

4.2.

4.3.

surface free from pin holes/ scaling/ pitting/surface corrosions and care to be taken noto go too deep nor more than 1.0 papers proceeding paper. Once the Grinding steps are completed, the area is ready for Polishing.

Polisher Using Lavigated(i.e. 6Once the polishing steps are completed, the area is ready for

locations as per table. Refer page 5 and 6.

approximately three times the size of the area to be replicated, is held by tweezers and softened on one side only. Apply acetone with an eyedropper, allow to set for approximately 30 seconds, and thenthen pressed firmly against the area with the eraser end of a pencil or tip of the fingers and helped several seconds. Care must be taken that the acetate is not allowed to slip or a smudged replica will hardens, usually 10 to 15 minutes, depending upon the size of the replica. Once it has hardened it can be stripped with tweezers. At this point the stripped replica should be put into a separatedoubleappropriately.



4.1. SCOPE

To Examine

Naya Nangal, by

4.2. APPARATUS & MATERIALS: Metallurgical Microscope. Hand Grinding Machine Portable Polishing Machines & Diamond Paste Etching Reagents as per table Replica Kit Polishing papers, sylvet cloth, polishing media, thermo setting or therm

4.3. SPECIMEN PREPARATION TECHNIQUE Grinding

surface free from pin holes/ scaling/ pitting/surface corrosions and care to be taken noto go too deep nor more than 1.0 papers (80- Grit To 1proceeding paper. Once the Grinding steps are completed, the area is ready for Polishing.

PolishingPolisher Using Lavigated(i.e. 6-micron diamond compound followed by 1Once the polishing steps are completed, the area is ready for

Etching locations as per table. Refer page 5 and 6.

Replication approximately three times the size of the area to be replicated, is held by tweezers and softened on one side only. Apply acetone with an eyedropper, allow to set for approximately 30 seconds, and thenthen pressed firmly against the area with the eraser end of a pencil or tip of the fingers and helped several seconds. Care must be taken that the acetate is not allowed to slip or a smudged replica will hardens, usually 10 to 15 minutes, depending upon the size of the replica. Once it has hardened it can be stripped with tweezers. At this point the stripped replica should be put into a separatedouble-sided tape. Several Replicas should be made of each area and should be labelled appropriately.




To Examine the microstructure of the

by the Insitu

APPARATUS & MATERIALS:Metallurgical Microscope.Hand Grinding MachinePortable Polishing Machines & Diamond PasteEtching Reagents as per tableReplica Kit Polishing papers, sylvet cloth, polishing media, thermo setting or therm

SPECIMEN PREPARATION TECHNIQUE Grinding –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 noto go too deep nor more than 1.0

Grit To 172 proceeding paper. Once the Grinding steps are completed, the area is ready for

Polishing - Wash the sample thoroughly anPolisher Using Lavigated

micron diamond compound followed by 1Once the polishing steps are completed, the area is ready for

Etching – to etch the reagents in the mirror finished surface of the test required locations as per table. Refer page 5 and 6.

Replication – 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. Apply acetone with an eyedropper, allow to set for approximately 30 seconds, and thenthen pressed firmly against the area with the eraser end of a pencil or tip of the fingers and helped several seconds. Care must be taken that the acetate is not allowed to slip or a smudged replica will hardens, usually 10 to 15 minutes, depending upon the size of the replica. Once it has hardened it can be stripped with tweezers. At this point the stripped replica should be put into a separate contain

sided tape. Several Replicas should be made of each area and should be labelled appropriately.




the microstructure of the

Insitu-Metallograph

APPARATUS & MATERIALS: Metallurgical Microscope. Hand Grinding Machine Portable Polishing Machines & Diamond PasteEtching Reagents as per table

Polishing papers, sylvet cloth, polishing media, thermo setting or therm

SPECIMEN PREPARATION TECHNIQUE 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 noto go too deep nor more than 1.0

Grit Paper)should be done in a particular direction to that of proceeding paper. Once the Grinding steps are completed, the area is ready for

Wash the sample thoroughly an Aluminium oxide Suspension or Magnesium oxide Suspension


to etch the reagents in the mirror finished surface of the test required locations as per table. Refer page 5 and 6.

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. Apply acetone with an eyedropper, allow to set for approximately 30 seconds, and thenthen pressed firmly against the area with the eraser end of a pencil or tip of the fingers and helped several seconds. Care must be taken that the acetate is not allowed to slip or a smudged replica will be obtained. Let the replica remain in this position until it hardens, usually 10 to 15 minutes, depending upon the size of the replica. Once it has hardened it can be stripped with tweezers. At this point the stripped replica should be

container (usually a small Plastic boxsided tape. Several Replicas should be made of each area and should be labelled




the microstructure of the fertilizer unit @

Metallography.

Portable Polishing Machines & Diamond PasteEtching Reagents as per table


SPECIMEN PREPARATION TECHNIQUE - 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 noto go too deep nor more than 1.0 mm from

Grit Paper)should be done in a particular direction to that of proceeding paper. Once the Grinding steps are completed, the area is ready for

Wash the sample thoroughly anAluminium oxide Suspension or Magnesium oxide Suspension


to etch the reagents in the mirror finished surface of the test required locations as per table. Refer page 5 and 6.

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. Apply acetone with an eyedropper, allow to set for

shake to remove excess acetone. 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. Care must be taken that the acetate is not allowed to slip

be obtained. Let the replica remain in this position until it hardens, usually 10 to 15 minutes, depending upon the size of the replica. Once it has hardened it can be stripped with tweezers. At this point the stripped replica should be

er (usually a small Plastic boxsided tape. Several Replicas should be made of each area and should be labelled




fertilizer unit @

Portable Polishing Machines & Diamond Paste


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 no

mm from surface. GrindGrit Paper)should be done in a particular direction to that of

proceeding paper. Once the Grinding steps are completed, the area is ready for

Wash the sample thoroughly and finally polish by the Portable Aluminium oxide Suspension or Magnesium oxide Suspension

micron diamond compound followed by 1-micron diamond compound polish). Once the polishing steps are completed, the area is ready for

to etch the reagents in the mirror finished surface of the test required




er (usually a small Plastic box, or taped to a glass slide with sided tape. Several Replicas should be made of each area and should be labelled



REPORT No: MT /

fertilizer unit @ National Fertilizers Limited,



surface. Grind the surface with emery Grit Paper)should be done in a particular direction to that of


d finally polish by the Portable Aluminium oxide Suspension or Magnesium oxide Suspension

micron diamond compound polish). Once the polishing steps are completed, the area is ready for Etching.





, or taped to a glass slide with sided tape. Several Replicas should be made of each area and should be labelled




National Fertilizers Limited,

Polishing papers, sylvet cloth, polishing media, thermo setting or thermo plastics.


the surface with emery Grit Paper)should be done in a particular direction to that of



micron diamond compound polish).






5 of 27

SBI /001

National Fertilizers Limited,

o plastics.

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

the surface with emery Grit Paper)should be done in a particular direction to that of



micron diamond compound polish).






4.

5


.4 PROCEDURE Examination

400X 500X andbe made.

Examine the replicated Specimen in Metallurgical Microscope under 100 X & higher magnification for the following.

o Microstructureo Condition of Metalso Grain Sizeo Decarburization if anyo Internal Granular Cracks if anyo Any other Micro Defects.

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

5 RESULT (observation and recommendation)

In many spots no microstructural deformation observed Some spots having

these spots need inspection after 20,000 hours of operation For detailed



PROCEDURE – EXAMINATION OF REPLICAExamination of replica carried out with the Metallurgical Microscope at 100 X & 400X 500X and photographs can be taken and also semi quantitative evaluations can

Examine the replicated Specimen in Metallurgical Microscope under 100 X & higher

ation for the following.MicrostructureCondition of MetalsGrain Size Decarburization if anyInternal Granular Cracks if anyAny other Micro Defects.


observation and recommendation)

In many spots no microstructural deformation observedSome spots having precipitates these spots need inspection after 20,000 hours of operation

detailed observation and recommendation refer page no. 7



EXAMINATION OF REPLICAof replica carried out with the Metallurgical Microscope at 100 X &

photographs can be taken and also semi quantitative evaluations can

Examine the replicated Specimen in Metallurgical Microscope under 100 X & higher ation for the following.

Microstructure Condition of Metals

Decarburization if any Internal Granular Cracks if anyAny other Micro Defects.


observation and recommendation)

In many spots no microstructural deformation observedprecipitates

these spots need inspection after 20,000 hours of operationobservation and recommendation refer page no. 7



EXAMINATION OF REPLICA of replica carried out with the Metallurgical Microscope at 100 X &

photographs can be taken and also semi quantitative evaluations can


Internal Granular Cracks if any

The Microphotographs can be taken for any of the above features, if desired on

observation and recommendation) :

In many spots no microstructural deformation observedprecipitates along grain boundary.




of replica carried out with the Metallurgical Microscope at 100 X & photographs can be taken and also semi quantitative evaluations can



In many spots no microstructural deformation observed.grain boundary.







. grain boundary. Creep damage

these spots need inspection after 20,000 hours of operations. observation and recommendation refer page no. 7-27







Creep damage - class 2


6 of 27




class 2. In


Sport details

S.NO

1

2

3

4

S.NO

1

2

3

S.NO

1

2

3

4

5

6

7

8

9

10

11

12

13


rt details:

DIRECTON

NORTH

NORTH

SOUTH

TOP

DIRECTION

NORTH

SOUTH

NORTH

TUBE NO

8

17

25

34

2

15

24

39

6

8

10

30

40



DIRECTON

NORTH

NORTH

SOUTH

TOP

DIRECTION

NORTH

SOUTH

NORTH

TUBE NO DIRECTION



LOCATION

BELOW TUBE NO 25

BELOW TUBE NO 10

BELOW TUBE NO 6

NEAR TUBE NO 22 TOP SIDE

RAISER TUBE

FIT BOTTOM TO TOP

DIRECTION

NORTH

SOUTH

SOUTH

NORTH

NORTH SOUTH

SOUTH

NORTH

NORTH

SOUTH

SOUTH

SOUTH

NORTH



HEADER

LOCATION

BELOW TUBE NO 25

BELOW TUBE NO 10

BELOW TUBE NO 6

NEAR TUBE NO 22 TOP SIDE

RAISER TUBE

FIT BOTTOM TO TOP

7

7

1

TUBES

FIT BOTTOM TO TOP



NEAR TUBE NO 22 TOP

ROW

FIT BOTTOM TO TOP 10

14

15

11

9

9

10

10

7

1

7

7

9



ROW

A

B

C

C

ROW

A

B

C

ROW

A

A

A

A

B

B

B

B

C

C

C

C

C




PAGE NO

8

9

10

11

PAGE NO

12

13

14

PAGE NO

15

16

17

18

19

20

21

22

23

24

25

26

27


7 of 27

PAGE NO

PAGE NO

PAGE NO

15

16

17

18

19

20

21

22

23

24

25

26

27


Microstructure

HEADER


Microstructure:

HEADER –A ROW NEAR TUBE NO 25 NORTH



A ROW NEAR TUBE NO 25 NORTH



A ROW NEAR TUBE NO 25 NORTH



A ROW NEAR TUBE NO 25 NORTH SIDE



100 X, Etched

400 X, Etched




100 X, Etched

Observation:

Microstructure shows

*

*

* Precipitates observed along grain boundry.

Creep damage

Recommendation:

Reafter 20 000 hservice

400 X, Etched




Observation:


* Austenite matrix

* No Crack


Creep damage

Recommendation:

Re-inspection after 20 000 hservice

8 of 27


Observation:


Austenite matrix.


Creep damage - class 2

Recommendation:

inspection to be done after 20 000 hours of

insitu metallograhy report

Engineering