An Evaluation of Testing Methods to

Detect Surface Iron Contamination

by David Frey

Iron contamination on the internal surfaces of Zr

process equipment can cause serious corrosion
problems.
This presentation will focus on various common testing
methods to detect iron and will evaluate the effectiveness of
those tests along with the hazards associated with their use.
Sources of iron contamination and methods of removal will
also be discussed.

Two common methods, Ferroxyl and Copper Sulfate will be

compared to a very simple water test.
Common sources of iron contamination will be discussed along
with methods of iron removal and prevention.

Corrosion Solutions Conference 09

Unplanned Iron Detection Test SS Expansion Joint

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Why Worry About Iron Contamination?

Zr is vulnerable to ferric chloride pitting attack. Surface
iron in a chlorine environment such as HCl can result in
severe pitting of Zirconium and possible SCC.

Residual embedded iron is less likely to cause pitting or corrosion

attack in process applications involving Nitric, sulfuric or acetic
acid. However Iron contamination should always be avoided or
removed.
Surface iron contamination is usually not a problem for Titanium
except for concentrated hot brine applications. As a precaution,
obvious iron contamination should by removed.

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Sources of Iron
Contamination:

Forming: Rolling, Head Forming

(spinning/pressing.
Fixtures & Tooling
Grinding
Iron dust
Blasting (iron contamination in sand)
Handling fork lifts, trucking chains
Tube Expansion (roller expanding)
Hydrotesting (rust deposits from water
supply (fire hydrants).

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Common Testing Methods to Detect Surface Iron

Ferroxyl Testing
ASTM A380
ASTM B912 (modified)
ASTM B650 App. X1
AMS 2700 method 103
Copper Sulfate
AMS 2700 method 102
ASTM B650 7.4.3
Alternate Methods
Water AMS 2700
Head and Shoulders

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Ferroxyl Testing:

Add nitric acid to distilled water and then

add potassium ferricyanide in the following proportions.
Distilled water
Nitric Acid (60-67%)
Potassium ferricyanide

94 weight %
3 weight %
3 weight %

1 gal
1/5 pt.
30 g

1000 cubic cm
20 cubic cm
4 oz

Apply solution with plastic or glass spray atomizer

The appearance of a blue stain within 15 seconds of application is evidence
of iron contamination.
Flush surface with water as quickly as possible after inspection to rinse off
test solution. White vinegar or 5-20 weight % acetic acid may also be used.
Rinse solution should be collected for proper disposal.

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Copper Sulfate:

Dissolve 8 g of copper sulfate in 500 ml

of distilled water, to which 2-3 ml of concentrated sulfuric acid has
been added.
Apply solution with plastic or glass spray atomizer. Re-spray as required
to keep the surface wet for a period of 6-7 minutes.
Wipe the surface dry and visually inspect for areas of deposited copper. A
copper deposit will indicate the presence of iron.
Flush surface with water after inspection to rinse off test solution.
Rinse solution should be collected for proper disposal.

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Testing Precautions:
Ferroxyl
Potassium ferricyanide is not a dangerous poison as are the simple cyanides.
However, the solution can emit highly toxic cyanide fumes if heated to
decomposition or mixed with concentrated acid.
Rubber gloves and face shields should be used.
Avoid inhalation of atomized spray.
Not recommended for use on equipment intended for food processing or
pharmaceuticals.
Solution and rinse water must be disposed of as hazardous waste.

Copper Sulfate
Rubber gloves and face shields should be used.
Avoid inhalation of atomized spray.
Not recommended for use on equipment intended for food processing or
pharmaceuticals.
Solution and rinse water must be disposed of as hazardous waste.

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Test Protocol
Test subject was Zr 702
elliptical head (warm formed
by spinning)
PVC spill containment
One half of the ID surface of
the head received additional
surface conditioning by
grinding to provide a
reasonably smooth surface.
The other half was as
received from the head
forming company and had a
sandblasted surface profile.

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Test Protocol head was divided into 6 pie shaped sections. The as
blasted half had 3 sections, one each, for Ferroxyl, Copper Sulfate and
water. The half with additional surface grinding preparation was divided
in the same manner.

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Test Protocol Ferroxyl, Copper Sulfate and water were sprayed onto the
divided sections of each half. Adjacent sections were covered with
plastic to prevent overspray.

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Test Results Ferroxyl

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Test Results Copper Sulfate

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Test Results Plain Old Water

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Test Results Side by Side Comparison note the streaks of embedded

iron from the head spin forming die. Embedded iron was readily detected
with Ferroxyl and water methods.
Ferroxyl

Water

Copper Sulfate

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Test Results unexpected crack indications revealed by Ferroxyl.

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Test Results Detection of iron dust on the surface, Ferroxyl only

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Observations and Conclusions from test results

Ferroxyl Method demonstrated the best sensitivity and
detection capability.
Water testing was sufficiently capable of detecting iron
small enough to be of concern for FeCl pitting.
Copper Sulfate was not much better than water testing
and any residual copper that is not removed could cause
a problem with Cupric chlorides.

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Practical Recommendations
Water testing method is sufficient for detecting iron in less critical
applications where FeCl pitting is not a major concern. Or for
intermediate testing prior to a final ferroxyl test prior to shipment.
Water testing can be a cost effective method for large vessels and
columns where Ferroxyl would be very expensive and hazardous.

End Users and Fabricators need to work together to determine the

need for iron detection inspection and develop a practical
inspection plan. The risks of iron contamination exist throughout
the fabrication process and expensive tests such as ferroxyl should
not be performed too early in the process.
Inspect after forming / prior to any HT / after hydrotesting

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Removal of Iron Contamination

Nitric Pickle

Mechanical Grinding

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Prevention of Iron Contamination
Production work areas should be divided so that fabrication is
confined to an area with only one grade of material.
Material should be protected from handling equipment such as
chains, hooks, fork lifts.
Forming equipment should be ground or wiped clean prior to any
forming or rolling. Pre-clean internal metal surfaces.
Hand tools and brushes should be segregated by materials.
Fixtures should have SS contact surfaces.
Personnel should avoid walking on process surfaces
Blasting sand should be iron free.
Hydrotest water should be filtered.

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Conclusions:

Testing for iron contamination is an important part of the

fabrication/inspection process.
The Method of Iron Detection Testing should be based on
the process application of the equipment and any
processing (such as heat treatment) that is performed
during fabrication.
The sequence of testing and fabrication operations should
be carefully planned in order to minimize cost and to be
confident that the equipment did not become
contaminated prior to shipment.