ISO /DIS 8407

DRAFT IN TERN ATION AL STAN DARD

ISO/ DIS

84 07

Metals

and

alloys

Procedures

for

removal

of

corrosion products from corrosion test specimens

1 S c o p e a n d fi e l d o f a p p l i c a t i o n
1 . 1 T h i s I n t e r n a t i o n a l S t a n d a r d s p e c i fi e s
for the procedures for the removal of
corrosion products formed on metal and
alloy corrosion test specimens during
t h e i r ex p o s u r e i n c o r r o s i v e e n v i r o n m e n t s .
1 . 2 T h e p r o c e d u r e s s p e c i fi e d a r e d e s i g n e d
to remove corrosion products without
s i g n i fi c a n t r e m o v a l o f b a s e m e t a l . T h i s
allows an accurate determination of the
mass Ioss of the metal or alloy which
o c c u r r e d d u r i n g ex p o s u r e t o t h e c o r r o s i v e
environment.
1.3 These procedures, in some cases, may
apply
to
metal
coatings.
However,
p o s s i b l e e ff e c t s f r o m t h e s u b s t r a t e m u s t
be considered.
2 Procedures
2.1 Corrosion product removal procedures
can
be
divided
into
three
general
categories:
chemical,
electrolytic
and
mechanical.
2.1.1 An ideal procedure should remove
o n l y c o r r o s i o n p ro d u c t s a n d n o t r e s u l t i n
removal
of
any
base
metal.
To
determinate the mass loss of the base
metal when removing corrosion products,
replicate uncorroded control specimens
should be cleaned by the same procedure
as
used
on
the
test
specimen.
By
weighing the control specimen before and
a ft e r c l e a n i n g ( w e i g h i n g t o t h e fi ft h
s i g n i fi c a n t
fi g u r e
is
suggested),
the
ex t e n t
of
metal
loss
resulting
from
cleaning can be utilized to correct the
corrosion mass loss.

2.1.2 The procedure given in 2.1.1 may

not be reliable for cases where heavily
corroded specimens are to be cleaned.
The
application
of
replicate
cleaning
procedures to specimens with corroded
s u r f a c e s w i l l o ft e n , e v e n i n t h e a b s e n c e o f
corrosion products, result in continuing

mass
losses.
This
is
because
a
corroded surface, particularly of a
multiphase
alloy,
is
o ft e n
more
susceptible that, a new machined or
polished surface to corrosion by the
cleaning procedure. In such cases, the
following method of determining the
mass
loss
due
to
the
cleaning
procedure is preferred.
2.1.2.1 The cleaning procedure should
be repeated on specimens several
times.
The
mass
loss
should
be
d e t e r m i n e d a ft e r e a c h c l e a n i n g b y
w e i g h i n g t h e s p e c i m e n ( t o t h e fi ft h
s i g n i fi c a n t fi g u r e i s s u g g e s t e d ) .
2.1.2.2 The mass Ioss should be
showed or a graph as a function of the
number of equal cleaning cycles (see
t h e fi g u r e ) . Tw o l i n e s w i l l b e o b t a i n e d
AB and BC. The latter will correspond
t o c o r r o s i o n o f t h e m e t a l a ft e r r e m o v a l
of corrosion product. The true mass
loss due to corrosion will correspond
to
the
point
D
obtained
by
ex t r a p o l a t i o n t o z e r o t i m e o f t h e l i n e
BC.
When the cleaning method does
not corrode the metal, the line BC will
be horizontal and the true mass loss
will be that represented by point B
since D will have the value of B.
2.1.2.3
To
minimize
uncertainty
associated with corrosion of the metal
by the cleaning method, a method
should be chosen to provide the lowest
slope (near to the horizontal) of line
BC.
2 . 1 . 3 Re p e a t e d t h e t r e a t m e n t m a y b e
required
for
complete
removal
of
corrosion products.
2.1.2.1.
2.1.4 All
prepared

cleaning solutions shall be

with
distilled
water
and

reagent grade chemicals.

2.1.5 Any cleaning procedure should
be followed by a thorough rinsing of

1) W henever distilled water is required in this specif ication, deionized water with a conductivity less than 20 Siemens/cm may be used

ISO /DIS 8407

the test specimen with distilled water and
immediate drying.
2 . 2 C h e m i c a l p r o c e d u r e o n l y ex p o s u r e o f
t h e c o r r o s i o n t e s t s p e c i m e n i n a s p e c i fi c
chemical solution which is designed to
remove

the

corrosion

products

with

minimal dissolution of any base metal.

Several procedures are listed in the
a n n ex .
WA R N I N G t h e s e m e t h o d s m a y b e
hazardous to personnel. They should
n o t b e c a r r i e d o u t b y i n ex p e r i e n c e d
employees
or
without
professional
supervision.

2.2.1 Chemical cleaning is often preceded by

light brushing of the test specimen to remove
loose, bulky corrosion products.

method is recommended. The mechanical

forces used to cleaning should be held as nearly
constant as possible.

2.2.2 Intermittent removal of specimens from

the chemical solution for light brushing can
often facilitate the removal of tightly adherent
corrosion
products.
2.2.3 Chemical cleaning also is often followed
by light brushing to remove loose products.

3 Test report
Reports of results shell include the following
information:
a) Reference to this International Standard;

2.3 Electrolytic cleaning also can be utilized for

removal of corrosion products. Several useful
methods for corrosion test specimens of iron,
cast iron or steel are given in the annex.
Electrolytic cleaning should be preceded by
brushing of the test specimen to remove loose,
bulky corrosion products. Brushing also should
follow the electrolytic clearing to remove any
loose slime or deposits. This will help to
minimize any redeposition of metal from
reducible corrosion products which would
reduce the apparent mass loss.
2.4 Mechanical procedures can include
scraping,
scrubbing,
brushing,
ultrasonic
methods, mechanical shock, and impact
blasting (grit blasting. water-jet blasting, etc.)
These methods are often utilized to remove
heavily encrusted corrosion products. Scrubbing
with a bristle brush and mild abrasive/distilled
water slurry can also be used to remove
corrosion products.
Vigorous mechanical cleaning will result to the
removal of some base metal, so care should be
exercised. These methods should be used only
when others fail to provide adequate removal of
corrosion products. As with, other methods,
correction for metal boss doe to the cleaning

b) The procedure utilized in the removal of

corrosion products following corrosion testing;
c) For chemical procedures, the composition
and concentrations of chemicals employed, the
solution temperature and duration of cleaning;
d) For electrolytic procedures, the composition
and concentrations of chemicals employed the
solution temperature, the anode material and
current density, and duration of cleaning;
e) For mechanical procedures, the specific
mechanical method (bristle brush scrubbing,
wooden scraper, etc.) employed, any abrasive
compounds utilized, and duration of cleaning;

f) Where multiple procedures are used, the

appropriate details for each method and the
sequence of methods;

g) The results from cleaning of controls (see

2.1.1) or from repetitive cleaning steps (see
2.1.2) designed to assess mass loss from
removal of base metal during to cleaning
process.

Mass loss

C
B

Number of clearing cycles

ISO /DIS 8407

Figure

Mass loss of corroded specimens resulting from repetitive cleaning cycles

Annex
Chemical and electrolytic cleaning procedures for removal of
corrosion products
(This annex does not form part of the standard.)

A.0 Introduction
In the development of this international Standard, a number of sources were consulted to identify
chemical and electrolytic cleaning procedures. This annex summarizes the results of this survey.

A.1 Procedure
Tables 1 and 2 summarize various chemical and electrolytic cleaning procedures for removal of corrosion
products. The specific choice of procedure for a given material will depend on many factors including
previous experience. This international Standard should be consulted for guidance in the proper
application of the procedure in tables 1 and 2.
For all the cleaning procedures listed, it la suggested that surfaces to be cleaned of corrosion products be
maintained vertical. This will minimize retention of any gases released during the cleaning procedure at
horizontal surfaces which in turn may alter the uniformity of the cleaning process.

ISO /DIS 8407

Table 1 Chemical cleaning procedures for removal of corrosion products

Designati
on

C.1.1

Material
Aluminium
and
aluminium
alloys

Chemical
50 ml phosphoric acid
(H3P04, = 1,69 g/ml)
20 g chromium trioxide (CrO3)
Distilled water to make 1000
ml

Time

Temperature

5 to 10 min

90C
Boiling

1 to 5 min

20 to 25C

1 to 3 min

20 to 25C

1 to 3 min

20 to 25C

1 to 3 min

20 to 25C

5 to 10 sec

20 to 25C

30 to 60min

40 to 50C

1 to 25 min

20 to 25C

Nitric acid (HN03, 1,42 g/ml )

C.1.2

C.2.1

Copper
and copper
alloys

C.2.2

C.2.3

C.2.4

C.2.5

c.3.1

Iron and
steel

C.3.2

500 ml hydrochloric acid

(HCI, = 1,19 g/ml)
Distilled water to make 1 000
ml
4,9 g sodium Cyanide (NaCN)
Distilled water to make 1000
ml
100 ml sulfuric acid
(H2 SO4, =1,84 g/ml)
Distilled water to make 1000
ml
120 ml sulfuric acid
(H2S04, = 1,84g/ml)
30 g sodium dichromate
(Na2Cr2O7.2H20)
Distilled water to make 1000
ml
54 ml sulfuric acid
(H2S04, = 1,84g/ml)
Distilled water to make 1000
ml
1000 ml hydrochloric acid
(HCI, = 1,19 g/ml)
20 g antimony trioxide (Sb2O3)
50g stannous chloride (SnCl2)
50g sodium hidroxide (NaOH)
200 g granulated zinc or zinc
chips
Distilled water to make 1000
ml
200g sodium hidroxide
20 g granulated zinc or zinc
chips
Distilled water to make 1000
ml

C.3.3

C.3.4

200 g diammonium
citrate[(NH4)2HC6H5O7]
Distilled water to make 1000
ml

C.3.5

500 ml hydrochloric acid

(HCI, = 1,19 g/ml)
3.5 g hexamethylene tetramine
Distilled water to make 1000
ml

C.4.1

C.4.2

C.4.3

Lead and
lead alloys

10 ml acetic acid
(CH3COOH)
Distilled water to make 1000
ml
50 g ammonium acetate
(CH3COONH4)
Distilled water to make 1000
ml
250 g ammonium acetate
(CH3COONH4)
Distilled water to make 1000
ml

30 to 40 min

80 to 90C

30 to 40 min

80 to 90C

20 min

75 to 90C

10 min

20 to 25C

5 min

Boiling

10 min

60 to 70 C

5 min

60 to 70 C

Remarks

If corrosion product films remain, then

follow with nitric acid procedure below.

Remove extraneous deposits and bulky

corrosion products to avoid reactions that
may result in excessive removal of base
metal.
De- aeration of solution with purified
nitrogen will
minimize
base
metal
removal.
Remove copper sulfide corrosion products
which may not be removed by above
hydrochloric acid treatment.
Remove bulky corrosion products before
treatment to minimize copper redeposition
on specimen surface.

Removes redeposited copper resulting

from sulfuric acid treatment.
De aerate solution with nitrogen.
Brushing of test specimens to remove
corrosion
products
followed
by
reinmersion
for
3
to
4
sec
is
recommended.
Solution should be vigorously stirred or
specimen should be brushed. Longer times
may be required in certain instances.
Caution should be excercised in the used
of any zinc dust since spontaneous
ignition upon exposure to air can occur.

Caution should be excercised in the used

of any zinc dust since spontaneous
ignition upon exposure to air can occur.

Longer times may be required in certain

instances.

ISO /DIS 8407

Table 1 (Continued)

Designation

C.5.1

Material
Magnesium
and
Magnesium
alloys

Chemical
100 g ml Chromiun trioxide
(CrO3)
10 g silver nitrate(AgNO3)
Distilled water to make 1000
ml

Time

Temperature

1 min

Boiling

1 min

20 to 25C

1 to 3 min

20 to 25C

1 to 3 min

20 to 25C

20 min

60C

10 to 60 min

70 C

5 min

60 C

5 min

Boiling

5 to 20 min

20 to 25C

20 min

Boiling

10 min

Boiling

Remarks

The silver salt is present to precipitate

chloride.

200 g Chromiun trioxide (CrO3)

10 g silver nitrate(AgNO3)
C.5.2

20 g barium nitrate [Ba(NO3)2]

Distilled water to make 1000
ml
Nickel and
Nickel alloys

C.6.1

C.7.1

Stainless
steels

C. 7.2

100 g citric acid (C6H8O7)

50 ml sulfuric acid
(H2S04, = 1,84g/ml)
2 g inhibitor (diorthotoly
thlourea or quinoline
ethyliodide or naphtholquinoline)
Distilled water to make 1000
ml

C. 7.3

200 g sodium hydroxide (Na

OH)30 g potassium
permanganate (KMnO4)
100 g diammonium citrate
[(HN4)2HC6H5O7]
Distilled water to make 1000
ml

C. 7.4

100 ml nitric acid

(HNO3, = 1,19 g/ml)
20 ml hydrofluoric acid
(HF, = 0,987 g/ml)
Distilled water to make 1000
ml

C. 7.5

200g hydroxide sodium

(NaOH)
50 g zinc powder
Distilled water to make 1000
ml

C.7.6

C.8.1

150 ml hydrochloric acid

(HCI, = 1,19 g/ml)
Distilled water to make 1000
ml
100 ml sulfuric acid (H2 SO4,
=1,84 g/ml)
Distilled water to make 1000
ml
100 ml nitric acid
(HNO3, = 1,42 g/ml)
Distilled water to make 1000
ml
150g diamonium citrate
[(HN4)2HC6H5O7]
Distilled water to make 1000
ml

Tin and Tin

alloys

150 g trisodium phosphate

(Na3PO4.12H2O)
Distilled water to make 1000
ml

The barium salt is present to precipitate

sulfate.

Caution should be excercised in the

used of any zinc dust since spontaneous
ignition upon exposure to air can occur.

C.8.2

ISO /DIS 8407

50 ml hydrochloric acid
(HCl, =1.19 g/ml)
Distilled water to make 1000
ml

C. 9.1

Zinc and
Zincs Alloys

150 ml ammonium hydroxide

(NH4OH), =0.90 g/ml)
Distilled water to make 1000
ml
Followed by
50 g Chromiun trioxide (CrO3)
10 g silver nitrate(AgNO3)
Distilled water to make 1000
ml

10 min

20 C

5 min

20 to 25C

15 to 20 sec

Boiling

The silver nitrate should be dissolved in

water and added to the boiling chromic
acid to prevent excessive crystallization
of silver chromate. The chromic acid
must be sulfate free to avoid attack of
zinc base metal.

Table 1 (concluded)
Designation

Material

C.9.2

C.9.3

Chemical
100 g
ammonium chloride
(NH4Cl)
Distilled water to make 1000 ml
200 g Chromiun trioxide (CrO3)
Distilled water to make 1000 ml

Time

Temperature

2 to 5 min

70 C

1 min

80 C

15 sec

20 to 25 C

5 min

20 to 25 C

2 to 5 min

70 C

C.9.4
85 ml hydriolic acid
(Hl, = 1.5 g/ml)
Distilled water to make 1000 ml
100 g ammonium acetate
[(HN4)2S2O8]
Distilled water to make 1000 ml
100 g ammonium acetate
[CHOONH4]
Distilled water to make 1000 ml

C.9.5
C.9.6

Remarks

Chloride contamination of the

chromic acid from corrosion
products formed in salt
environments should be avoided
to prevent attack of the zinc base
metal.
Some zinc base metal may be
removed. A control specimen (see
2.1.1.) should be employed.
Particularly recommended for
galvanized steel.

Table 2 Electrolityc cleaning procedures form removal of corrosion

products
Designation
E.1.1

Material
Iron,
Cast Iron,
steel.

Chemical
75
g
sodium
hidroxide
(NaOH)
25 g sodium sulfate(Na2SO4)
75
g
sodium
carbonate(Na2SO4)
75
g
sodium
carbonate( Na2CO3)
Distilled water to make 1000
ml

Time

Temperature

Remarks

20 to 30
min

20 to 25 C

Cathodic Treatment with 100 to

200 A/m2 current density. Use
carbon, platinum or stainless
steel anode.

3 min

75 C

Cathodic Treatment with 2000

A/m2 current density. Use
carbon, platinum or lead anode.

5 min

20 to 25 C

3 min

75 C

E.1.2
28 ml sulfuric acid
(H2SO4, = 1.84 g/ml)
0.5 g inhibitor(diorthotoly
thlourea or quinoline
ethyliodide or naphtholquinoline)
Distilled water to make 1000
ml

E.1.3

100 g diammonium citrate

{(NH4)2HC6H5O7)}
Distilled water to make 1000
ml

E.2.1

Lea and lead alloys

28 ml sulfuric acid
(H2SO4, = 1.84 g/ml)
0.5 g inhibitor(diorthotoly
thlourea or quinoline
ethyliodide or naphtholquinoline)

Cathodic Treatment with 100

A/m2 current density. Use
carbon or platinum anode.
Cathodic Treatment with 2000
A/m2 current density. Use
carbon, platinum or lead anode.

ISO /DIS 8407

Distilled water to make 1000
ml

E.3.1

E.4.1

E.4.2

Copper and copper

alloys

Zinc and cadmium

7.5 g potasium chloride (KCl)

Distilled water to make 1000
ml
50
g
sodium
hydrogenphosfhate (Na2HPO4)
Distilled water to make 1000
ml
100 g sodium hydroxide
(NaOH)
Distilled water to make 1000
ml

1 to 3 min

20 to 25 C
Cathodic Treatment with 100
A/m2 current density. Use
carbon or platinum anode.

5 min

70 C

1 to 2 min

20 to 25 C

Cathodic Treatment with 110

A/m2 current density. Specimen
shall be energized prior to
inmersion. Use carbon,
platinum or stainless steal
anode.
Cathodic Treatment with 100
A/m2 current density. Specimen
shall be energized prior to
inmersion. Use carbon,
platinum or stainless steal
anode.