Surface Characterization Techniques

• A: Scanning Probe Method

• B: Low Energy Scattering
• C: Near Surface Method
• D: Analytical Methods in Electron Microscopy
 The optical microscope
A light microscope used visible light and a
system of lenses to magnify images of small
samples.
The maximum normal magnifications of the
ocular and objective are 10× and 100×
respectively, giving a final magnification of
1,000×.
 Surface Characterization Techniques
• Optical microscope
• Electron microscope
– SEM. (scanning electron microscope); produces images
of a sample by scanning it with a focused beam
of electrons. The electrons interact with atoms in the
sample, producing information about the sample's
surface topography with magnification 0 to 500,000
times.
• Field Emission Scanning Electron Microscopy
(FeSEM). provides topographical and elemental
information at magnifications of 10x to 300,000x,
with virtually unlimited depth of field. Compared
with convention scanning electron microscopy
(SEM), (FESEM) produces clearer, less
electrostatically distorted images with spatial
resolution down to 1 1/2 nanometers – three to six
times better.
 Energy dispersive spectroscopy (EDS)
• identifies the elemental composition of materials
imaged in a scanning electron microscope for all
elements.
• Applications:
• Materials evaluation and identification
• Failure analysis
• Quality control screening
• Material verification
• Plating specification and certification
 X-ray Diffraction Analysis
http://www.academia.edu/5547134/X-ray_Diffraction_Analysis_Principle_Instrument_and_Method

• X-ray powder diffraction (XRD) is a rapid

analytical technique primarily used for
phase identification of a crystalline
material and can provide information on
unit cell dimensions. The analyzed
material is finely ground, homogenized,
and average bulk composition is
determined.
 Analytical Methods in Electron Microscopy

Energy-Dispersive Spectrometry (EDS)

 Auger electron spectroscopy (AES
An analytical technique to study surfaces. IT is a
widely used surface analysis technique that has
been successfully applied to many diverse fields
ranging from gas phase chemistry to
nanostructure characterization.
 Raman spectroscopy
Technique used to observe vibrational,
rotational, and other low-frequency modes in a
system. Raman spectroscopy is commonly used
in chemistry to provide a fingerprint by which
molecules can be identified.
Raman gas analyzers have many practical
applications. For instance, they are used in
medicine for real-time monitoring of anesthetic
and respiratory gas mixtures during surgery.
 Scanning Probe Techniques

• a: Scanning Probe Techniques

 Near Surface Methods
• c: X-Ray Photoelectron Spectroscopy (XPS)
using soft x-ray (200-2000 eV) radiation to examine core-levels

a sampling depth on the order of 5 nm.

 Surface Crystallography
Higher-Miller-Index Crystal Planes
Surface Defects:
Typical results of FeS by SEM
 Corrosion Monitor Comparison
Electro- TXINS
Coupon ER Ultrason
Feature LPR Chemic FSM-IT Monitorin
s Probes ic Scan
al Noise g System
All except high
Service Conductive Conductive
All All All All O2
Environments Aqueous Aqueous
environments
Presence of
No No Yes Yes No No No
Electrolyte

Area of Coverage Point Point Point Point Point/Section Point/Section Section

Pigging
No No No No Yes Yes Yes
Compatible
Continuous
No Yes Yes Yes No Yes Yes
Monitoring
Satellite
No No No No No Yes Yes
Communication
Cost to Production
High High High High Minimal Minimal None
from Shutdowns

Cost of Equipment Low Medium Medium High High High Medium

Labor Cost to
Low Medium Medium Medium High High Medium
Install
Labor Cost to
High High High High High Low Low
Repeat
 Applications
Any metal substrate where hydrogen is being produced as a result of the corrosion process.

• Pipelines (Sour) • Pipelines (Natural Gas)

• Pipeline (Sweet) • Pipelines (Condensate)
• Gas Plants • Treaters
• Water Disposal • Vessels
• Petrochemical • Amine Towers
• Water Floods • Refinery
• Closed or Sealed Rolling Stock (rail cars or tanker
trucks)
 Applications
Gas and Oil Production (H2S)

• Oil/Gas Gathering and Transmission Lines

• Oil/Gas Well Heads

• Sour Water Flood Lines

• Underground Gas Storage Facilities

 Applications
Gas-Oil Separation Plants and Gas
Plants (H2S)
• Amine Units – Inlets, • Sour Gas Gathering
Outlets, transfer lines Lines
• Contactors • Fractionators
• Absorbers • Catalytic Cracker –
• Flash Drums overhead recovery
system
• Wash Columns and
Drums • Hot Wells
• Blow down Drums • High and Low pressure
sour gas separators
• Flare Lines
• Sour Water Strippers
 Applications
Refinery HF Alkylation Units

• Acid Settler Tanks

• Accumulators
• Condensors
• Depropanisers
• Transfer Lines
• Recontactors
 Installation of the
Equipment

• Site preparation – hand tool only to white metal

• Bonding the vessel to the pipe - Liquid epoxy
• Mechanically clamp the vessel to the pipe
• Mount monitoring equipment to a pole above
ground or to secured area on the rolling stock
 Reporting

• Graphical representation of corrosive activity

• Programming alarms can be set by Client

• All client information is password protected for

their use only
Graph Showing 2 Corrosion Events

ABC Co.

2nd Event
1st Event
 Pressure

-80
-70
-60
-50
-40
-30
-20
-10
0
7/17/2007
7/18/2007
7/19/2007
7/20/2007
7/21/2007
7/22/2007
7/23/2007
7/24/2007
7/25/2007
7/26/2007
7/27/2007
7/28/2007
7/29/2007
7/30/2007
7/31/2007
8/1/2007
8/2/2007
8/3/2007
8/4/2007
8/5/2007
8/7/2007
8/16/2007

Re-evacuate
8/17/2007
8/18/2007
8/19/2007
8/20/2007
8/21/2007
Re-evacuate

8/22/2007
8/23/2007
8/24/2007
8/25/2007
8/26/2007
8/27/2007
8/28/2007
8/29/2007

Daily Readings
8/30/2007
Re-evacuate

8/31/2007
9/1/2007
9/2/2007
Customer #2

9/3/2007
9/4/2007
9/5/2007
FIGURE 3 - Pressure Readings from 7/16/07 to 9/24/07

9/5/2007
9/5/2007
Re-evacuate

9/6/2007
9/7/2007
9/8/2007
9/9/2007
9/10/2007
9/11/2007
9/12/2007
9/13/2007
9/14/2007
9/15/2007
9/16/2007
9/17/2007
9/18/2007
9/19/2007
9/20/2007
9/21/2007
Re-evacuate

9/22/2007
9/23/2007
Re-evacuate

9/24/2007
 Customer #2
TABLE 3 - Average Vacuum Loss Over Time

25

20
Average Change in Pressure

15

10

0
July 23 - 29 July 30 - Aug 5 Aug 16 - 22 Aug 24 - 28 Aug 29 - Sept 5 Sept 6 - 18 Sept 19 - 21 Sept 22 - 24
 Benefits

• Real time data

• Records
• Non-intrusive
• Low maintenance
• Remote capability
• Coordinates corrosion programs
• Cost effective
 Benefits (cont.)

• No down time
• Works in Conjunction with other Technologies
• Early Corrosion Detection
• High Risk Remote Areas Can be Monitored
• Low Installation and Operating Costs
• High Temperature Installations (200˚C)
“Can be placed on higher temperature if welded”
 Limitations of the Technology

• No correlation of TXINS data to intrusive probes or

corrosion coupons

• Does not work in fully oxygenated water systems or

ponds

• Each system has to be looked at individually, no

comparison
 Commonly Asked Questions and
Answers

Q1: Does your Hydrogen Vessel work in Sweet and

Sour Gas Systems?
A1: Yes
 Thank You

• Q AND A
Immersed test
Salt spry chamber
Outdoor corrosion
SCC
Crevice corrosion test