This presentation is the intellectual property of UltraClean Electropolish, Inc.

Do not reproduce in part or in whole without prior written authorization of UltraClean Electropolish, Inc. 03-01-06

Optimization of High Purity Product

Contact Surfaces on Nickel Alloys
via Electropolishing
R. Keith Raney

R. Keith Raney
Has been active in electropolishing since 1975 when he and
his family started the first electropolish company in the
southern US.
Developed on site electropolishing in the petro-chemical
facilities in Texas.
Worked extensively with nuclear industry electropolishing
recirculation piping systems and reactor containments.
Developed procedures for electropolishing 20 stainless steel
tubing for semi-conductor industry.
Designed, Installed, and trained several US based vessel
manufactures electropolish systems.
Active member of ASTM BPE since 2001.

20Ra

Do You Think This Surface is

Easier to Clean or..

20Ra

Would This Surface Be

Better?
4

Surface Roughness
The previous two slides both measure 20 Ra.
To achieve this I had the electropolished
coupon sanded to and 80 grit (35 Ra) then
electropolished to the 20Ra seen.
20 Ra mechanically polished coupon was
sanded to a 180 grit.
The purpose is to illustrate that Ra is not as
critical to performance as is the microsurface finish!

2B Sheet
Metal
10
Ra
,
10 Ra 2B Sheet Metal
1500X

How About This

vs. ..
1000 X
1000 X
6

2B Electropolished 7Ra,
5Ra

2B
Electropolish
1500X

This?
7

Mechanical Polishing -Sanding

To achieve a specified Ra on product contact surfaces most

fabricated products must receive some form of mechanical
sanding, grinding, or polishing.

Mechanical Polishing -Sanding

MILL FINISH - Hot Rolled Annealed 316 Plate Material

Most alloy plate material used in fabrication is purchased in this

condition.

120 Ra
9

Mechanical Polishing Sanding

SEM 1500X 180 grit 304 Stainless Steel

25 Ra
All mechanical operations impart a finish similar to the
surface shown here.
10

Mechanical Polishing - Sanding

Ra 11.5uin

11

Mechanical Polishing -Sanding

Mechanical Polishing/Sanding/Grinding to
achieve a specific Ra will cause a damaged
layer and/or heat effected zone (Bielby
Layer) to be produced.

Mechanical Polishing -Sanding

This damaged layer will include material smeared over
impurities such as:

Abrasive material/compounds
Iron or other contamination from handling/forming
equipment
Paint, dye, grease, adhesives

Mechanical finishing operations all cause damage to the

material for some depth below the surface. The depth of
this damage will vary depending on how aggressively the
material was worked.

The Bielby Layer

Mechanical finishing is performed to achieve required Ra on
metal
surfaces will result in crystal fractures and other structural
changes.
These conditions allow the formation of surface corrosion
cells.
This condition is known as the Bielby layer.

Electropolishing can completely remove this

damaged layer which is believed to be the biggest
contributure to rouge formation in WFI systems.
14

J. Wulff illustrates this damage on honed, ground, and

electropolished samples of 18-8 CrNi.
On the honed sample a layer of Austenite and Cold Deformed Ferrite sits atop of a
layer of Cold Deformed Ferrite to a depth of 5 m (.00002). The ground sample had
seven distinct layers of non-austenite material atop the pure stainless.
The seven layers top to bottom;
7. Oxide (0-5m)

6. Deformed Oxide with Grit Inclusions (5-18m)

.001

5. Deformed Austenite (18-22m)

4. Cold Deformed Ferrite and Deformed Austenite
(22-25m)
3. Cold Deformed Ferrite (25-29m)
2. Austenite and Cold Deformed Ferrite (29-34m)
= (.00134)
1. Austenite only

HONED GROUND
GROUND E-POLISH
E-POLISH
HONED

15

Electropolishing

Electropolishing
Why Bother?

Why Bother?

Damaged Layer Bielby Layer

.0003

180 grit sanded surface

180 Grit -Electropolished

The damage in the uppermost grains

can be seen here after sanding.

Once electropolished the damaged

layer is removed leaving undistorted
metal crystal structure at the surface
17

ELECTROPOLISH
The Ultimate Product Contact Surface!
Electropolishing provides optimum microsurface finish!
Electropolishing provides the minimum total
surface area!
Electropolishing provides pure alloy without
contamination or damage at the materials
surface (product contact interface)!

18

ELECTROPOLISH
The Cleanest Surface Possible
Electropolished alloy surfaces offer optimum
cleanability!
Electropolished alloy surfaces offer optimum
sterility!
Electropolished surface offers optimum
resistance to corrosion for any given alloy!
Electropolished surface offers rouge
formation resistance when base material
condition is the cause!
19

Vocabulary

Electropolish: the electrolytic removal of metal in a highly ionic solution

by means of electrical potential and current.

Anode: the work piece, part, or component connected to the positive

side of a DC power source that becomes a sacrificial anode when the part
is exposed to the electropolish process

Cathode: the necessary conductor that is connected to the negative side

of a DC power source and is present in the circuit during the
electropolishing process

Electrolyte: An acid blend into which the work piece is placed for
processing. The bath is the ionic solution which wets the work piece and
carries the metal ions from anode to cathode.

20

Electropolishing; How it Works

A surface to be
electropolished is made
anodic (+) in a DC power
circuit
The work is then
exposed to an acid
electrolyte (dipped or
wetted)
A cathode (-) is present
adjacent to the portion
of the work that requires
electropolishing

21

Electropolishing; How it Works

22

Electropolishing; How it Works

When the power is applied an anodic film forms on the surface of the work
and the material begins to be removed ion by ion
The effect on the microscopic surface is to smooth and level as the
microscopic peaks dissolve more rapidly than the microscopic valleys due
to the increase in resistance to current flow as the film get thicker in the
valleys

23

Electropolishing; How it Works

When the process is allowed to continue for an adequate amount
of time the surface becomes microscopically smooth and
virtually featureless
As the anodic film becomes uniform in thickness the benefits of
electropolishing have been accomplished and material will
continue to be removed uniformly until the process is stopped

24

Electropolishing; How it Works

MILL FINISH - Hot Rolled Annealed 316 Plate Material

120 Ra
25

Electropolishing; How it Works

As Electropolishing Exposure Increases Microscopic Smoothing Continues
Until Optimum Improvement is Achieved

26

Electropolishing; How it Works

ELECTROPOLISHED - Hot Rolled Annealed 316 Plate Material

35 Ra
27

On Site (In Situ) Electropolishing

Electropolish equipment purchased without the
finish, a capitalized value added service.
Remediation of poor or damaged factory
electropolished equipment.
WFI System Vessels electropolished to control
rouge formation and re-deposition on loop
components.
Autoclaves, sterilizer trays, parts washers, steam
traps, lyo trays can all be electropolished to
remove steam rouge and retard reformation.

In Situ Remediation

Shop Repair
After Mechanical Polish & EP

Before Mechanical Polish &

EP

Remediation instead of replacement!

In this case 12 vessels were returned

to service saving $M in replacement.

Field Repair
Magnetic agitator damage

Repaired agitator damage

Optimized Micro Surface &

Surface Area Reduction

Electropolishing offers a microscopic featureless

surface.
Electropolishing offers a total surface area that has
been dramatically reduced.
The only comparable surface finish on metal is
produced by lapping as on metallurgical samples,
and gage blocks.
35

2B Stainless Sheet Metal

SEM 1500X 304 Stainless Steel

Note the cross section in the following slide to see

illustration of surface roughness
36

2B Stainless Sheet Metal

White Light Interfermetric Surface Analysis

Ra 7.4uin

Observe this cross section

37

#4 Stainless Sheet Metal

SEM 1500X 180 grit 304 Stainless Steel

38

#4 Stainless Sheet Metal

Ra 11.5uin

39

Electropolished Stainless Coupon

SEM 1500X - 304 Stainless Steel

40

Damaged Layer Bielby Layer

.0003

180 Grit -Electropolished

180 grit sanded surface

41

Electropolished Stainless Sheet Metal

Ra 2.3uin

Compare this to previous slides

42

Bacterial Control
The Cold Worked, Damaged, or Beibly layer offers significant site for
bacterial adhesion and bio-film formation.

Bacterial bio-films can contribute to corrosion as they can breakdown the

passive film underlying the formations.

If the bio-film is then successfully removed an active site (nonpassivated) can allow corrosion to initiate via a galvanic effect.

NO ELECTROPOLISH

ELECTROPOLISHED

43

The disks were placed in 100 mL purified water, autoclaved for 1

hour, brought to room temperature and water supplemented to
100 mL. These procedures were repeated 50 times.

Multiple imaging techniques demonstrate the manipulation of surface to

reduce bacterial contamination and corrosion
J.W. Arnold, D.H. Booth, O. Suzuki, & G. W. Bailey Journal Of Microscopy, Vol. 216, Pt 3 Dec. 2004

45

Bacterial Control
Bugs like to hide and form colonies

From: Edstrom Industries, Inc. (Update7)

46

Bacterial Control
Electropolishing eliminates the hideouts

From: Edstrom Industries, Inc. (Update7)

47

Ra How Important Is It?

Ra is the most important thing to me
(famous engineer)

20 Ra mech. Polish

20 Ra Electropolished

Both surfaces shown here measure 20Ra.

Which surface is best for high purity applications?
48

49

Electropolishing VS. Buffing

Although similar in appearance; buffing should never be allowed to be the
final surface finish on product contact surfaces.

Embedded aluminum- oxide

abrasive residue

Buffed

Electropolished
50

ASME BPE-2007

ASME BPE-2007

ASME BPE-2009
The latest revision of the BPE standard will include:
NONMANDATORY APPENDIX H
ELECTROPOLISHING PROCEDURE QUALIFICATION
Which defines a method for qualifying the
electropolish process used for electropolishing
component(s) surfaces that will be exposed to the
product(s) in bioprocessing, pharmaceutical, and
personal care products systems and ancillary
equipment

ASME BPE
The ASME BPE Committee Meetings will be held January 1821 at the Rio Mar Hotel. Participation by Bio-Pharm
Manufactures is always encouraged.
Wednesday (1/20) 1:00 PM -3:00PM a white paper will be
presented;

Determining Acceptable Levels of Weld Discoloration on Mechanically Polished

and Electropolished Surfaces
By: Ken Kimbrel
Abstract: This paper will identify acceptable levels of weld discoloration on
mechanically polished and electropolished surfaces and also show proven shop and
field remediation practices to removes excessive heat tint. Additionally, we will
show the effect of various oxygen levels and its contribution to heat tint as well as
impact on corrosion resistance. The information herein is based on actual field
experiences and successful methods of field remediation.

Qualifying Vendors
End users are encouraged to develop a program for
qualifying an electropolish vendor.
A good electropolish vendor should be able to produce a
procedure for the process used, including independent
verification that the procedure used is capable of
producing the desired improvements to the micro-surface
that have been described during this presentation.
Featureless micro-surface
Removal of damaged / heat affected zone
Optimized corrosion resistance

55

Buffing Looks Good

Buffing is used to make a component look bright and
mirror like. Unfortunately this practice is often used to
make equipment required to be electropolished look
cosmetically more appealing or to touch up
electropolished surfaces.

Buffing offers no improvement in corrosion

resistance

Buffing will in all cases embed grease, adhesives, and

any other dirt present under a layer of smeared
and torn material.
56

Buffing is Not Good

When a high purity surface is required buffing should

never be used.
Proper electropolishing over buffing will remove
completely any reflectivity achieved making the practice
unnecessary

End users should insist no buffing be

performed on any product contact surfaces.

57

Buffing
Electropolishing
Buffedvs.
either
side of
final weld appears
white where surface
damaged by chloride
exposure NOTE:
Electropolished
surfaces above and
below buffed area
unaffected by
corrosion!

Buffing vs. Electropolishing AL6XN

58

New vessel VP-3200 during fabrication, dimpled cooling jacket shown

Top head to sidewall weld

New vessel VP-3200, AL6XN, far wall from manway, June 2006

Electropolishing; How it Works

61

Rouge
Rouge is a naturally occurring phenomenon in Stainless Steel
high purity water or pure steam systems. The degree to
which it forms depends upon:
(a) The stainless steel material used for each component
within the system.
(b) How the system was fabricated; i.e. welding, surface
finish, passivation treatment.
(c) What process service conditions the system is exposed to;
i.e. water purity, process chemicals, temperatures, pressures,
mechanical stresses, surface velocity and oxygen exposure.
(d) How the system is maintained.

FeO Hematite Type II Rouge

Typical Rouge is caused by hot purified water or clean steam exposure.

FeO Hematite Type II Rouge

Corrosion damage from concentrated chloride exposure over many years.

FeO Magnetite or Type III Rouge

Believed to have been caused in WFI system running 90C water. Not
removed during typical de-rouging procedure.

Spray Ball Rouge

Rouge

Rouge is corrosion! Sometimes staining from product manufacturing is

mistaken for rouge.

Rouge indicates the passive layer has been compromised!

Rouge can become loose particles that move throughout the system.
Once mobile the rouge particles may be considered an additive which is
prohibited by FDA requirements.

Rouge can dramatically effect surface roughness: In a recent field

observation on a consistently rouged non-electropolished PW vessel
surface roughness Ra readings were observed as high as 90Ra when read
on the rouged surface, following rouge removal the same surface
measured < 20Ra.

67

Rouge Control
Proper Electropolishing has been proven very effective in
slowing the formation of rouge on 316 stainless steel surfaces.

Electropolishing allows the product contact surfaces to be free

of the physical and metallurgical damage (Bielby layer) that
takes place during mechanical polishing that can significantly
contribute to rouge formation.

The use of Electropolished surfaces in wet processing areas

could retard the effects of rouging and corrosion on stainless
steel components (Arnold, Booth, Suzuki, & Bailey Journal of Microscopy Dec. 2004)

68

Case Study 1 - Rouge Control

In WFI systems all 316 stainless steel exposed to the high purity
water should be properly electropolished to insure complete
removal of any damaged layer from mechanical polishing.

In this hot WFI vessel the band and bottom

head were electropolished 30 months ago
no rouge here, yet reformed everywhere else!

69

Case Study WFI Systems

These vessels and entire loop have never required derouging or passivation since being Electropolished!

Case Study WFI System Tanks

Two WFI (80C) vessels 36,000L & 20,000L both with a 180
grit factory interior finish and a history of rouging required
chemically cleaned and (citric) passivated every 12 months.
The owner had the vessels completely electropolished in
situ over the original 180 grit factory finish followed by
(citric) passivation.
After 4 years in service the owner reported that no derouging and passivation had been required as no rouge has
returned in the entire system!
One time Electropolishing cost $50K* per vessel eliminating
cost of yearly cleaning and passivation as had been routine.
* CAPITOLIZED Average cost per vessel (size & conditions will impact actual charges)

71

Electrochemical Cleaning (ECC)

The same techniques used to provide spot electropolishing
can be used as a extremely effective cleaning / de-rouging
process.
Much faster than complete electropolishing, electrochemical
cleaning has proven very effective in removing;
Product residue resistant to conventional cleaning
Staining from SIP operations
Grey residue in non-electropolished equipment
Rouge from WFI Systems, Clean Steam Systems,
Autoclaves, Parts Washers, and related equipment.
Electrochemical Cleaning like electropolishing removes
material from the surface being cleaned with no risk of
damage!
72

Surface Comparison Study

Mech. Polish

Electrochemical
Cleaned

Mech. Polish &

Passivate

Electropolished

Electrochemical Cleaning (ECC)

This technique is an extremely effective process. It utilizes
specifically formulated abstraction chemistry in conjunction
with electrolysis. To some degree it replicates
electropolishing however it is a process that removes only
the readily soluble passive film contaminates such as iron,
nickel, aluminum (grinding residue, etc.)

ASTM B 912 Standard Specification for Passivation of

Stainless Steels using Electropolishing recognizes both ECC
and electropolishing as a suitable form of passivation as
long as a citric acid or nitric acid flush proceeds final rinsing
and drying.

Chemical Passivation
Chemical passivation procedures require first cleaning and de-rouging
then introduction of nitric acid or citric acid to remove free iron. If citric
acid is used in order for the surface to form a passive layer it must be
exposed to an oxidizer or allowed to dry and be exposed to oxygen for
several hours. If nitric acid (oxidizer) is used the oxygen is produced
when the acid comes in contact with the stainless steel and no extended
dry period is necessary as the passive film is already established.

Electropolishing & ECC liberates oxygen during the operation on the

metals surface which provides, like nitric acid an simultaneous passive
layer. Following electropolishing or ECC the surface simply needs to be
flushed with a room temperature citric or nitric acid to remove any
residual acid salts.

Electropolishing or ECC components can be passivated as part of a

system without risk of damage unlike some chemical cleaning that may
use strong etching agents as part of the cleaning process.

Standard Cleaning and Passivation

Treatment Process
DI Water Flush
Derouging with Organic Acid Intensifiers and Reducing
Agents (phase optional based on presence of rouge)
High Purity Water Rinse
Decontamination with Alkaline and/or Detergents
High Purity Water Rinse
Citric/Chelant or 20% Solution Nitric Acid Passivation
High Purity Water Rinse
Oxidizer or Sanitization with Peroxides (Citric process only)
Final High Purity Water Rinse

Field Assembled New System

Passivation - Yes or No?
Even if the components are passivated or electropolished
at the factory this is an essential step on new systems.
The Cr/Fe ratio Must be >1.5 for best corrosion resistance
performance once in service.
Field assembled systems usually include Orbital Welds
which in the as welded condition have Cr/Fe Ratios of 0.11
Plus High Manganese + Silicon
Unless the Cr/Fe Ratio is increased and the Mn + Si is
reduced, The corrosion resistance will be poor on these
welds.
Installation practices can introduce contaminates in
components, plus the presence of field welds make final
cleaning and passivation of the entire system essential
before placing the system into service.

Weld Seam Analysis Before Passivation

Heat Affected Zone
80
70
60
50
OXYGEN

40
IRON

30
CHROMIUM

20
10
0
9

Article By: K. Balmer

millimeters

Weld Seam Analysis After Passivation

Heat Affected Zone

80
70
60
50
OXYGEN
IRON
CHROMIUM

40
30
20
10
0

Article by: K. Balmer

millimeters

ESCA Tests on 316L Passivation Time

Passivation Systems: Commercial Citric Acid system

Performed on Weld of 316L EP Tubing

Passivation versus Time

1.8

Chromium / Iron R atio

1.6

1.4

1.2

0.8

0.6

0.4

0.2

10.00

30.00

60.00

Time in Minutes

120.00

240.00

81

Conclusions
1. Mechanical Polishing including buffing, even if cleaned and passivated can be
a source of product contamination from the manufacturing process, bacterial
contamination due to surface profiles that can harbor bio-films making them
very difficult to remove, easily form rouge when exposed to high purity water
(PW,WFI) or clean steam.
2. Surface roughness (Ra) is not a suitable method of specifying product contact
surfaces.
3. Proper Electropolishing offers the optimum product contact surface as it;
3.1 Removes damaged surface layer present after mechanical polishing or
sanding.
3.2 Removes any embedded abrasive or metallic residue present after mechanical
polishing or sanding.
3.3 Provides a microscopic featureless surface that offers best resistance to
bacterial contamination, corrosion, rouge formation, product residue retention.
3.4 Allows for an extremely uniform passive layer with no thin spots for
failure.

Conclusions
4. Passivation is a naturally occurring process on stainless steel that can be
accelerated in its formation and potentially enhanced in its Cr/Fe ratio with
Passivation processes including Electropolishing.
5. Electropolishing is an excellent passivation process that when properly
performed per ASTM B 912 requires no additional Passivation.

Referenced Specifications

ASTM A 380
Standard Practice for Cleaning, Descaling and Passivation of Stainless
Steel Parts, Equipment and Systems
ASTM A 967
Standard Specification for Chemical Passivation Treatments for
Stainless Steel parts
ISPE Baseline Pharmaceutical Engineering Guide, volume 4: Water and
Steam Systems
ASTM B 912-02
Standard Specification for Passivation of Stainless Steel Using
Electropolishing
Semi F19
Specification for the Surface Condition of the Wetted Surfaces of
Stainless Steel Components

Referenced Specifications(cont.)

European Hygienic Equipment Design Group Doc 18 Aug. 1998

Passivation of Stainless Steel R.R. Maller; 3-A and EHEDG

SAE AMS QQ-P-35 (Fed Std QQ-P-35C)

Passivation Treatments for Corrosion-Resistant Steel, Federal
Standard/Specification

MIL-STD-753C
Corrosion Resistant Steel Parts: Sampling, Inspection and Testing for
Surface Passivation

ASTM BPE-2009