Accred Qual Assur (2003) 8:235–241

DOI 10.1007/s00769-003-0624-x

Eugenija Ramoškienė Validation of salt spray corrosion test

Mykolas Gladkovas
Mudis Šalkauskas

Received: 14 September 2002
Accepted: 11 March 2003
Published online: 23 April 2003
© Springer-Verlag 2003
Presented at the Conference
“Metrology and Measurement – 2001”,
24–25 April 2001, Kaunas, Lithuania
E. Ramoškienė (✉) · M. Gladkovas
M. Šalkauskas
Institute of Chemistry,
Goštauto, 92600 Vilnius, Lithuania
e-mail: chemins@ktl.mii.lt; mudis@mail.lt
Abstract Quality control of corro-
sion test results implies the valida-
tion of the corrosion test method and
estimation of the uncertainty of cor-
rosion rate measurement. The corro-
sion test in an artificial atmosphere
of the salt spray mist needs evalua-
tion of corrosivity of the test cabinet
by reference specimens. Such cali-
bration of corrosion environment
raises very strict requirements for
the method description and details
of all procedures and used speci-
mens. Reliable corrosion measure-
ments by spray tests require valida-
tion of the experimental device to-
gether with the experimental proce-
dure and determination of corrosi-
vity uncertainty of the test cabinet
environment.
Corrosion tests have been con-
ducted for a long time but there are
only a few cases of corrosion data
quality assessment or interlaboratory
comparisons for such measurements.
Each test method when used in dif-
ferent laboratories gives different re-
sults, as it is impossible to perform
the whole procedure exactly in the
same manner. Therefore, a very es-
sential parameter of the method is its
robustness. A proper validation of
the corrosion test method means the
evaluation of the impact of various
environmental features and perfor-
mance variations on the uncertainty
of the test result.
Our aim was to present an experi-
mental evaluation of the corrosivity
of the salt spray corrosion test cabi-
net, to indicate the gaps in the de-
scription of the corrosion test meth-
od according to ISO 9227 and to es-
timate the main components of the
uncertainty of the corrosivity mea-
surement.
The validation results require
changes in the salt spray test method
description and maybe in the perfor-
mance.
Keywords Validation of method ·
Corrosivity · Measurement
uncertainty

Introduction The standard method for the test cabinet corrosivity

Corrosion tests in artificial atmospheres [1, 2, 3] are
used as comparative tests for the evaluation of corrosi-
vity of metals and metal alloys and corrosion protection
capability of various corrosion protection means by
metal plating, varnishing and paint coating as well as
anodic and conversion coating. Therefore, it is essential
to know precisely the corrosivity of the test cabinet en-
vironment.
determination is described in ISO 92271 [1] but we failed
to find any information about the validation of this meth-
od or its metrological parameter evaluation. On the other
hand, it is necessary to determine from the experimental
point of view whether this technique is reliable enough
as a standard method. A procedure is described in ISO
1 Translated and accepted as LST – national standard of Lithuania
Republic.
122 E. Ramoškienė · M. Gladkovas · M. Šalkauskas
5725-1 [4] for the estimation if the standard method is
sufficiently detailed and can possibly be improved.
ISO 9227 [1] does not specify in detail many neces-
sary parameters and does not determine the precision of
such a test method. The precision and accuracy of corro-
sion determination are influenced by many factors: prep-
aration of specimens, conditioning, removal of corrosion
products, cleaning, drying, etc. In literature on the corro-
sion tests we failed to find any information concerning
the quality of corrosion tests results. The aim of this pa-
per is to call attention to the problems in the corrosion
measurement data quality and the necessity to evaluate
the uncertainty for measurement results. We attempted to
show the main components of uncertainty of the result in
such a measurement on the basis of the experimental
evaluation of the corrosivity of the spray test corrosion
cabinet by means of reference specimens.
Materials and methods
An accuracy experiment can often be considered as a practical test of
the adequacy of the standard measurement method. One of the main
Table 1 Comparative analysis of standard LST ISO 92227:1997 and supplementary standards EN ISO 7384:1998 (1), LST ISO
7253:1998 (2) and possibilities of their experimental realization
Requirements of standard/reference methods
Corrosion cabinet
Cabinet capacity no less than 0.2 m3 and preferably
not less than 0.4 m3
At least two fog collecting devices in the zones
of the test specimens – glass cylinder with funnels
with a diameter of 100 mm
Inert plastic supports for the test specimens
Automatic registration of temperature and air humidity (1)
Determined humidity should be kept within ±5% (1)
If necessary, air circulation system shall be provided
Spraying device
Supply of clean air of controlled pressure [(70 to 170)±0.7] kPa
Air shall be humidified in saturation tower at temperature
several degrees higher than that of the cabinet
Level of the water must be maintained automatically
Atomizers shall be made of inert material
Adjustable baffles to obtain uniform distribution of the spray
Level of the salt solution shall be maintained automatically
Test solution
Sodium chloride (50±5) g in distilled or deionised water
with a conductivity not higher than 20 µS/cm at (25±2) °C
NaCl shall contain less than 0.001% of Ni, 0.001% Cu, 0.1%
of NaI and 0.5% (m/m) of total impurities; specific gravity range
of the solution is 1.0255 to 1.0400 and the pH range
within 6.0 to 7.0 at (25±2) °C
purposes of standardization is to eliminate differences between users
(laboratories) as far as possible and the data provided by the experi-
ment should reveal how effectively this purpose can be achieved.
According to the ISO 5725-1 requirements [4] a description of
the measurement method is one of the main sources of the uncer-
tainty and therefore it is essential for traceability of results. There-
fore, an analysis of the description of the standard test method was
performed and some ambiguous statements or lack of information
for experimental procedures were pinpointed as shortcomings. The
details of the experiment, which do not meet the requirements of
the description of the reference method, were marked off as well.
The result of these attempts is presented in Table 1.
Evaluation of cabinet corrosivity. In order to determine the cor-
rosivity of the corrosion cabinet environment eight tests were per-
formed [5] according to the standard method of the neutral salt
spray test (Table 1). The results of corrosion rate of RS and the
main statistical parameters such as the number of reference sam-
ples n, average RS mass m and RS mass loss ∆m of each RS, aver-
age RS surface area S and surface area of each RS Sn, mean aver-
ages of all eight experiments and their standard deviations are pre-
sented in Table 2a and 2b.
Corrosion rate values were calculated from the mass loss of
each test presenting a statistical array and indicating corrosion rate
ordered array average value ν, mode value νmode, median value
νmedian, and standard deviation s.
The statistical analysis of the data was performed for the deter-
mination of outliers by means of their interquartile range:
Peculiarities of the experimental device and procedures
and shortcomings in the standard
Cabinet capacity – 0.4 m3
Four collecting devices in the corners
PMMA plastic support for the five specimens
Not provided automatic registrationa
No data about humidity value
Not provideda
Compressed air pressure within determined interval,
and supplied without filtration
Not provideda
Provided
PMMA plastic
PMMA plastic
Maintained automatically
The test solution prepared from analytical grade NaCl
(GOST 4233-77); conductivity of deionised water not checked
Cu and Ni determined by AAS and both met the requirements
of ISO 9227; the pH of the prepared solution measured
with millivoltmeter pH-121