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 mass losses. This is because a

corroded surface, particularly of a
multiphase alloy, is o ft e n more
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 susceptible that, a new machined or
for the procedures for the removal of polished surface to corrosion by the
corrosion products formed on metal and cleaning procedure. In such cases, the
alloy corrosion test specimens during following method of determining the
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 .
mass loss due to the cleaning
procedure is preferred.
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
2.1.2.1 The cleaning procedure should
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
be repeated on specimens several
allows an accurate determination of the
times. The mass loss should be
mass Ioss of the metal or alloy which
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
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
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
environment.
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 ) .

1.3 These procedures, in some cases, may

2.1.2.2 The mass Ioss should be
apply to metal coatings. However,
showed or a graph as a function of the
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
number of equal cleaning cycles (see
be considered.
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
2 Procedures 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
2.1 Corrosion product removal procedures to the point D obtained by
can be divided into three general 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
categories: chemical, electrolytic and BC. When the cleaning method does
mechanical. not corrode the metal, the line BC will
be horizontal and the true mass loss
2.1.1 An ideal procedure should remove will be that represented by point B
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 since D will have the value of B.
removal of any base metal. To
determinate the mass loss of the base
2.1.2.3 To minimize uncertainty
metal when removing corrosion products,
associated with corrosion of the metal
replicate uncorroded control specimens
by the cleaning method, a method
should be cleaned by the same procedure
should be chosen to provide the lowest
as used on the test specimen. By
slope (near to the horizontal) of line
weighing the control specimen before and
BC.
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 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
cleaning can be utilized to correct the required for complete removal of
corrosion mass loss. corrosion products.

2.1.2.1.
2.1.2 The procedure given in 2.1.1 may 2.1.4 All cleaning solutions shall be
not be reliable for cases where heavily prepared with distilled water and
corroded specimens are to be cleaned. reagent grade chemicals.
The application of replicate cleaning
procedures to specimens with corroded
2.1.5 Any cleaning procedure should
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
be followed by a thorough rinsing of
corrosion products, result in continuing

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

1

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
2.2.1 Chemical cleaning is often preceded by
light brushing of the test specimen to remove
loose, bulky corrosion products.
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.
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
Mass loss
B
A
Number of clearing cycles
ISO /DIS 8407
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.
method is recommended. The mechanical
forces used to cleaning should be held as nearly
constant as possible.
3 Test report
Reports of results shell include the following
information:
a) Reference to this International Standard;
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.
C
2
 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.

3
 ISO /DIS 8407

Table 1 — Chemical cleaning procedures for removal of corrosion products

Designati
Material Time Temperature Remarks
on Chemical
Aluminium 50 ml phosphoric acid
and (H3P04, ρ= 1,69 g/ml)
aluminium 20 g chromium trioxide (CrO3)
C.1.1 90ºC If corrosion product films remain, then
alloys Distilled water to make 1000 5 to 10 min
Boiling follow with nitric acid procedure below.
ml

Remove extraneous deposits and bulky

Nitric acid (HN03, 1,42 g/ml )
corrosion products to avoid reactions that
C.1.2 1 to 5 min 20 to 25ºC
may result in excessive removal of base
metal.
Copper 500 ml hydrochloric acid De- aeration of solution with purified
C.2.1 and copper (HCI, ρ= 1,19 g/ml) nitrogen will minimize base metal
1 to 3 min 20 to 25ºC
alloys Distilled water to make 1 000 removal.
ml
4,9 g sodium Cyanide (NaCN) Remove copper sulfide corrosion products
C.2.2
Distilled water to make 1000 1 to 3 min 20 to 25ºC which may not be removed by above
ml hydrochloric acid treatment.
100 ml sulfuric acid Remove bulky corrosion products before
(H2 SO4, ρ =1,84 g/ml) treatment to minimize copper redeposition
C.2.3 1 to 3 min 20 to 25ºC
Distilled water to make 1000 on specimen surface.
ml
120 ml sulfuric acid
(H2S04, ρ= 1,84g/ml)
C.2.4 30 g sodium dichromate Removes redeposited copper resulting
5 to 10 sec 20 to 25ºC
(Na2Cr2O7.2H20) from sulfuric acid treatment.
Distilled water to make 1000
ml
54 ml sulfuric acid De – aerate solution with nitrogen.
(H2S04, ρ= 1,84g/ml) Brushing of test specimens to remove
C.2.5 Distilled water to make 1000 30 to 60min 40 to 50ºC corrosion products followed by
ml reinmersion for 3 to 4 sec is
recommended.
Iron and 1000 ml hydrochloric acid Solution should be vigorously stirred or
steel (HCI, ρ= 1,19 g/ml) specimen should be brushed. Longer times
c.3.1 1 to 25 min 20 to 25ºC
20 g antimony trioxide (Sb2O3) may be required in certain instances.
50g stannous chloride (SnCl2)
50g sodium hidroxide (NaOH) Caution should be excercised in the used
200 g granulated zinc or zinc of any zinc dust since spontaneous
C.3.2 chips ignition upon exposure to air can occur.
30 to 40 min 80 to 90ºC
Distilled water to make 1000
ml

200g sodium hidroxide Caution should be excercised in the used

20 g granulated zinc or zinc of any zinc dust since spontaneous
chips ignition upon exposure to air can occur.
C.3.3 30 to 40 min 80 to 90ºC
Distilled water to make 1000
ml

200 g diammonium
citrate[(NH4)2HC6H5O7]
C.3.4
Distilled water to make 1000 20 min 75 to 90ºC
ml

500 ml hydrochloric acid

(HCI, ρ= 1,19 g/ml)
C.3.5 3.5 g hexamethylene tetramine Longer times may be required in certain
10 min 20 to 25ºC
Distilled water to make 1000 instances.
ml

Lead and 10 ml acetic acid

lead alloys (CH3COOH)
C.4.1 5 min Boiling
Distilled water to make 1000
ml
50 g ammonium acetate
(CH3COONH4)
C.4.2 10 min 60 to 70 ºC
Distilled water to make 1000
ml
250 g ammonium acetate
(CH3COONH4)
C.4.3 5 min 60 to 70 ºC
Distilled water to make 1000
ml

4
 ISO /DIS 8407

Table 1 — (Continued)

Designation Material Chemical Time Temperature Remarks

Magnesium 100 g ml Chromiun trioxide
and (CrO3)
Magnesium 10 g silver nitrate(AgNO3)
C.5.1 The silver salt is present to precipitate
alloys Distilled water to make 1000 1 min Boiling
chloride.
ml

200 g Chromiun trioxide (CrO3)

10 g silver nitrate(AgNO3)

The barium salt is present to precipitate

C.5.2 20 g barium nitrate [Ba(NO3)2] 1 min 20 to 25ºC
sulfate.
Distilled water to make 1000
ml

Nickel and 150 ml hydrochloric acid

Nickel alloys (HCI, ρ= 1,19 g/ml)
1 to 3 min 20 to 25ºC
Distilled water to make 1000
C.6.1 ml
100 ml sulfuric acid (H2 SO4, ρ
=1,84 g/ml)
1 to 3 min 20 to 25ºC
Distilled water to make 1000
ml
Stainless 100 ml nitric acid
steels (HNO3, ρ= 1,42 g/ml)
C.7.1 20 min 60ºC
Distilled water to make 1000
ml
150g diamonium citrate
C. 7.2 [(HN4)2HC6H5O7]
Distilled water to make 1000 10 to 60 min 70 ºC
ml

100 g citric acid (C6H8O7)

50 ml sulfuric acid
(H2S04, ρ= 1,84g/ml)
2 g inhibitor (diorthotoly
thlourea or quinoline
C. 7.3 5 min 60 ºC
ethyliodide or β-
naphtholquinoline)
Distilled water to make 1000
ml

200 g sodium hydroxide (Na

OH)30 g potassium
permanganate (KMnO4)
C. 7.4 100 g diammonium citrate
5 min Boiling
[(HN4)2HC6H5O7]
Distilled water to make 1000
ml

100 ml nitric acid

(HNO3, ρ= 1,19 g/ml)
20 ml hydrofluoric acid
C. 7.5 (HF, ρ= 0,987 g/ml) 5 to 20 min 20 to 25ºC
Distilled water to make 1000
ml

200g hydroxide sodium

(NaOH)
Caution should be excercised in the
C.7.6 50 g zinc powder
20 min Boiling used of any zinc dust since spontaneous
Distilled water to make 1000
ignition upon exposure to air can occur.
ml

C.8.1 Tin and Tin 150 g trisodium phosphate 10 min Boiling

alloys (Na3PO4.12H2O)
Distilled water to make 1000
ml
C.8.2

5
 ISO /DIS 8407

50 ml hydrochloric acid
(HCl, ρ=1.19 g/ml)
Distilled water to make 1000 10 min 20 ºC
ml

150 ml ammonium hydroxide

Zinc and (NH4OH), ρ=0.90 g/ml) 5 min 20 to 25ºC
C. 9.1
Zincs Alloys Distilled water to make 1000
ml
Followed by

The silver nitrate should be dissolved in

50 g Chromiun trioxide (CrO3)
10 g silver nitrate(AgNO3)
Distilled water to make 1000
ml
15 to 20 sec Boiling 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 Chemical Time Temperature Remarks
100 g ammonium chloride
C.9.2 (NH4Cl) 2 to 5 min 70 °C
Distilled water to make 1000 ml
Chloride contamination of the
chromic acid from corrosion
C.9.3 200 g Chromiun trioxide (CrO3) products formed in salt
1 min 80 °C
Distilled water to make 1000 ml environments should be avoided
to prevent attack of the zinc base
C.9.4 metal.
85 ml hydriolic acid Some zinc base metal may be
(Hl, ρ= 1.5 g/ml) 15 sec 20 to 25 °C removed. A control specimen (see
C.9.5 Distilled water to make 1000 ml 2.1.1.) should be employed.
100 g ammonium acetate
Particularly recommended for
[(HN4)2S2O8] 5 min 20 to 25 °C
C.9.6 galvanized steel.
Distilled water to make 1000 ml
100 g ammonium acetate
[CHOONH4] 2 to 5 min 70 °C
Distilled water to make 1000 ml

Table 2 – Electrolityc cleaning procedures form removal of corrosion

products

Designation Material Chemical Time Temperature Remarks

E.1.1 75 g sodium hidroxide
Iron, (NaOH)
Cast Iron, 25 g sodium sulfate(Na2SO4)
steel. 75 g sodium
Cathodic Treatment with 100 to
carbonate(Na2SO4)
20 to 30 200 A/m2 current density. Use
75 g sodium 20 to 25 °C
min carbon, platinum or stainless
carbonate( Na2CO3)
steel anode.
Distilled water to make 1000
ml

E.1.2
28 ml sulfuric acid
(H2SO4, ρ= 1.84 g/ml)
0.5 g inhibitor(diorthotoly
thlourea or quinoline
Cathodic Treatment with 2000
ethyliodide or β-
3 min 75 °C A/m2 current density. Use
naphtholquinoline)
carbon, platinum or lead anode.
E.1.3 Distilled water to make 1000
ml

100 g diammonium citrate

{(NH4)2HC6H5O7)}
Cathodic Treatment with 100
Distilled water to make 1000
5 min 20 to 25 °C A/m2 current density. Use
ml
carbon or platinum anode.

28 ml sulfuric acid 3 min 75 °C Cathodic Treatment with 2000

(H2SO4, ρ= 1.84 g/ml) A/m2 current density. Use
0.5 g inhibitor(diorthotoly carbon, platinum or lead anode.
E.2.1 Lea and lead alloys thlourea or quinoline
ethyliodide or β-
naphtholquinoline)

6
 ISO /DIS 8407

Distilled water to make 1000

ml

7.5 g potasium chloride (KCl) 1 to 3 min 20 to 25 °C

E.3.1 Distilled water to make 1000 Cathodic Treatment with 100
Copper and copper
ml A/m2 current density. Use
alloys
carbon or platinum anode.

50 g sodium Cathodic Treatment with 110

hydrogenphosfhate (Na2HPO4) A/m2 current density. Specimen
E.4.1 Zinc and cadmium Distilled water to make 1000 shall be energized prior to
5 min 70 °C
ml inmersion. Use carbon,
platinum or stainless steal
anode.
100 g sodium hydroxide Cathodic Treatment with 100
E.4.2 (NaOH) A/m2 current density. Specimen
Distilled water to make 1000 shall be energized prior to
1 to 2 min 20 to 25 °C
ml inmersion. Use carbon,
platinum or stainless steal
anode.