MT-558 Corrosion Testing

• Introduction,
• Classification and purpose,
• materials and specimens,
• surface preparation,
• measuring and weighing,
• exposure techniques,
• environmental parameters,
• exposure time,
• laboratory tests,
• field tests and in-service tests,
• standard expressions for corrosion rates,
• evaluation of test damage,
• tests for different forms of corrosion,
• NACE test methods,
• linear polarization tests,
• AC impedence tests,
• presenting and summarizing data,
• interpretation of results.
Corrosion testing Philosophy
 Introduction
• No universal corrosion test
– exposure conditions
• metal
• environment
• Properly conducted corrosion tests inexpensive
• savings- avoid use of durable
– metal under unsuitable conditions efficient
– expensive material than necessary safe
• help in development of new better alloys
• Quality control corrosion tests
– acceptibility - must be rapid
• Tests durations- few hours to few years
• Planning needed- time
• Metallurgical, environmental, statistical variables
• interpretation of accelerated test results
 Test Objectives
• clearly define the test objectives-
– can be
– determining suitable material
– predicting service life
– new alloy/process evaluation
– materials development- for corrosion resistance
– Acceptance tests- QC
– Evaluation of environmental changes and effect of
inhibitors
– determine the most cost effective corrosion protection
method
– study of corrosion mechanisms
• Standardized tests and practices are
preferred
• when available
 R&D
• Research for alloy or process development
– how and why a particular form or mechanism of corrosion occurs
– Test methods may not always be standard
– electrochemical testing

small specimens and laboratory tests

simulated service tests

testing of actual parts

 Test Materials
• material representative of the current production.
– obtain fabrication history
– certified composition, hardness
– metallographic information
• metal forms in use-
– cast or wrought- process?
• Performance of one form does not guarantee same
performance in the other form
• forming- internal stresses- SCC, stress-induced IGC, surface
contamination prevents coatings
• machining- high T, contamination, active anions from EC
machining
• Welding- HAZ, flux residues, residual stress, filler metal, weld
spatter & oxides
• H.T.
 Test Specimen Preparation

• truly representative specimen

• shearing/stamping/cutting
– ex. sheared rolled sheet, extruded rod
machined slice
– surface preparation by machining or polishing,
chemical treatments- control necessary
– follow the standards
Nitrided steel
 Selection of corrosive media
• service performance
• field testing (actual environment)
• lab testing-
– when no past data, and frugal budget
– Environment reproduction
• [reactants, contaminants],
• T, pH, aeration,
• impingement, velocity,
• bacterialogical factors
 Accelerating tests
• faster tests always in demand
– how fast?
• until the corrosion mechanism (may be rxn)
remains the same
– eg. steel in water- can accelerate by T but
near boiling point, O is driven out => CR ↓.
 Reliability of corrosion test results
• usage of test results (numbers) led to undesirable
consequences
– reliability of test results is not good.
– difficult to get precise numbers that can be used in design or in
life prediction
– interpretation should be careful & realistic
• Corrosion rates: use with caution
– often
• short-term one-period exposure tests=> weight loss/exposure time,
determine a constant CR for a metal-environment combination, BUT
– mostly materials do not corrode linearly with time (corrosion
products influence!)
• Testing more specimens
– data scatter is common & inevitable
– scatter f ( specimen uniformity, surface condition, stability of test
environment)
• Precision-
– less in general, since corrosion systems are complex
– even less for localized corrosion- inhomogeneous μstructure
– unexpected results-
• schedule of inspection of specimen and environment helps
 In-service monitoring

• monitoring is important in design and

operation of modern industrial plants
– corrosion related concerns
• huge expenditures
• safety issues
– makes personnel aware of corrosion damage,
and rate of degradation
 Selection of a monitoring method
• ASTM G4 standard- exposing test coupons
• Other electrochemical methods
• Choice depends on
– purpose of the test
– cost
– more than one method gives confidence
– access to process streams
– response time
– safety- method should not be too intrusive
 Direct testing of Coupons
• Features
• Insert large # of coupons
– simultaneously
– to simulate different fabrication conditions eg welded, crevices
etc
• Actual process streams- synergistic effects of contaminants
– rider: process streams can get contaminated by coupons
• Monitoring of inhibitor programs
• Long exposure times- esp. good for localised corrosion
• Coupon design for specific corrosion form- crevice, pitting,
selective leaching etc.
• advantages vis-s-vis lab coupon tests
– large number of materials can be exposed,
simultaneously.
– corrosivity of process streams can be monitored
 Drawbacks of coupon testing
• cann’t detect rapid changes in corrosivity
– process upsets occur
• calculated CR is average over a period.
• electrochem. methods may be better
• no guarantee of localized corrosion before
coupon removal
• calculated CR of coupon can not be directly
translated in CR of equipment
– difficult to duplicate the equipment with a coupon
• mass is different
• coupon area:solution volume ratio
• correlation between ultrasonic thickness monitoring of
equipment and calculated CR of coupons are useful
• Certain forms of corrosion-
– eg erosion corrosion cann’t be simulated
• process turbulence is f(equipment design)
– Heat transfer effects: difficult to make/place coupons
eg. heat exchanger/condenser tubes
 Coupon Options-1

• Coupon design- v. important

– Uniform corrosion coupons
• rectangular sheet, stamped ID
– Coupon finish- should match w/ equipment,
costly
• mill finish, glass bead blasted, sand blasted,
abrasive cloth/paper sanded, machined,
electropolished
• edge preparation
– Galvanic corrosion coupons
• electrically coupled pair, 1:10 to 10:1 area
 Coupon Options-2
• Crevice corrosion coupons
• weld baking rings, flanged connections- common in
processes
• rubber bands, spot welded lap joints, wire wrapped around
threaded bolts, single/multiple crevice flat washers between
coupons
• Stress corrosion coupons
• residual stresses are common
• self-stressed bending specimens
• U-bend, cup impression, C-ring, welded panel
• crack forms and propagates without complete fracture
• Welded coupons
• weld bead, HAZ, residual stresses, sensitization,
• welded coupons
• Sensitized metals
• sensitized coupons
• AISI 316, sensitization HT: 650-700 °C, 30-40 minutes
 Test Racks
• simple hanging by insulated wire
• racks-
• large no. of specimens, firmly in place, isolated
– Spool (birdcage) rack: in open reactor vessels

– insert rack:
• pipe like units with flange way access
• equipment shutdown needed
– Slip-in rack
• equipment is in operation
• retraction chamber and gate valve
 Coupon Cleaning and Evaluation

• clean ASAP after removal

• weighing
• observation for localized corrosion
– naked eye, 30 to 50x microscope, SEM
– sometime bend and or section the coupon
and do metallographic observation
 Electrical resistance probes
• Instead of mass loss, measure the electrical resistance
of coupons
• wire or a suitable device
• corrosion decreases the C.S. and increases the R with
time
• R (corrosion) vs. t,
– slope gives corrosion rate
• Adv.
– small probes- easy installation
– continuous monitoring with PC
– most environments don’t affect the conductivity except molten
salts
• Disadv.
– potential leaks due to probe penetration
– temperature compensation device needed
– no information on localized attacks
Ultrasonic thickness Measurements
• in-situ technique,
– widely used
• transducer against vessel exterior
• series of measurements over a time interval
• minimum invasion
• Drawbacks
– cladded vessels- difficult
– high or low vessel temperatures make coupling
difficult
– overestimates thickness when remaining thickness is
approx. under 1.3 mm. 
Polarization Resistance Measurements
• estimate of corrosion rate
• Stern-Heary equation
• Icorr  =  (1/ Rp)  βaβc  /  (2.303 (βa+βc)  )  
• CR is inversely proportional to Rp
• Place the probe made of the material of interest,
where required in a plant
• Features
• +- 10mV
• instantaneous
• probe + PC with DAC systems
• alarms for very high CR
• Limitations:
• corroding environment must be electrolyte w/ low resistivity
• penetrate vessel wall- leaks!
• no info on localized corrosion
• CR values only approximate
• Suitable when CR changes are rapid
Measurement of corrosion potentials

• uncommon (Rp method better)

• useful for active-passive metals
– suddenly some process change (Cl-, or reducing
species) can cause transition from passive to active
state …..
• coupling of corrosion potential measurements w/
Rp method can confirm high CR.
• Rider: RE must be stable in long term
– environmental variables can make them unstable 
 AC Impedance Measurements
• same probes as used for Rp
• useful for high resistivity electrolytes
– steam condensate
– Rp will provide erroneously low Icorr
• Drawbacks
– Tafel slopes must be known to convert ac
impedance data into CR
– several hours to obtain full AC frequency
response curve
– Rp specimen designs are not optimized for ac
impedance analysis
 Hydrogen Probe
• H is a by-product of the corrosion reaction, in acidic
process environments
• Hydrogen can be absorbed by steel particularly when
traces of sulphide (prevents H recombination) or cyanide
are present.
– may lead to hydrogen induced failure by one or more of several
mechanisms.
• Concept:
– hydrogen probes detect the amount of hydrogen permeating
through the steel by mechanical (P chamber- monitor P) or
electrochemical measurement (oxidize outcoming H and
measure oxidation current)
• H amount – is a measure of corrosion rate- only relative
severity of corrosion damage
• Limitation:
– close to ambient T systems
– H diffusion rate should be high eg steel
• Gas pipelines- common application
• Adv.: no penetration of pipe wall
 Analysis of Process Streams
• presence of corrosion products
• routine sampling from the bottom of
distillation column
• AAS analysis for Fe, Cr, Ni
[Fe, Cr, Ni] α CR x Area of corroding metal,
if corrosion products are not precipitating &
if corrosion is the only source of elements

• Corrosion area may not be precise

– only relative results
– but help in knowing if the conditions improved
 Testing Procedure
• Selection and pretreatment of materials and test
specimens
• Surface preparation
• Measurement of surface area and thickness
• degreasing
• weighing-
• accuracy must correspond to expected weight loss
• masking
– wax, lacquer, paint, tape, glue, enamel
• exposure
– standardised racks with prescribed position and orientation
– In lab testins, environmental controls
• O2 conc (bubble air/O2/N2)
• pH, in long term testing
• T, Relative humidity in chambers, relative velocity between medium
and specimen
• Inspection: observation, weighing, thickness
measurements
• Determination of corrosion rate
????
 References
• ASM Handbook- Vol 9 Corrosion
• E. Bardal, Corrosion and Protection,
Springer, 2004, Chapter 9.