Methods of Compound Corrosion Test: Nissan Engineering Standard

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M0158 [2009-N]

Nissan Engineering Standard

NES Methods of Compound Corrosion Test

1. SCOPE
This Standard specifies the method to measure compound corrosion that uses the combined processes of salt
spraying or salt solution immersion followed by drying and moistening. The process will simulate and accelerate
corrosion of metal materials used on automobiles. Therefore this test will measure corrosion of metals of functional
decorative parts together with the coating effect of inorganic or organic plating of vehicle models.

2. SAMPLES

2.1 Test sample collection criteria


External surface samples shall be taken from the product part or the product itself. A representative sample may
be used where testing or evaluating the product itself is impractical. In this case samples shall be taken so that
they represent the product.

2.2 Shape, dimension and number of test samples


The test shall be performed on all products to which specification applies. When requirements have not been
specified, agreement between the parties concerned shall apply.

2.3 Preparation of test samples

2.3.1 Cleaning
Depending on the degree of dirt, samples shall be first immersed in an appropriate solvent such as ethyl alcohol
or acetone, and then the solvent shall be wiped off with a soft cloth. No corrosive solvents or substance that
coats the test sample materials, or substance that destroys protective coatings shall be used.

2.3.2 Primary damage to the samples


Depending on the purpose of the test, damage such as cross cutting, gravel or diamond shot may be inflicted on
the surface coating according to NES M 0007 “Testing Method for Automotive Paint”.

2.3.3 Protection of surfaces not used for testing


As a rule, any exposed original surface or end face of samples or products for testing other than the sections to
be tested shall be protected by appropriate coatings that are stable under the testing conditions. Surfaces not
included in the evaluation do not need to be protected, and this shall be agreed upon the parties involved.

2.3.4 Maintaining sample position


During the test, samples shall be kept in the testing chamber under the following conditions:

(1) Samples shall not touch any other parts other than the supporting frame.
(2) Samples shall not interfere with each other.
(3) Marks and holes for sample identification shall be made as close to the lower edge as possible.
To protect the holes on sample pieces for suspension, Item 2.3.3 above shall apply.

Furthermore, the tests including salt solution spraying (Methods I and IV) shall satisfy the following conditions:
(1) When testing the plate sample specified in Item 4.2 of NES M 0007, the plate shall be placed so that the main
face inclines 15° from the vertical line, and the plate shall be placed in the testing chamber so that it is not
orthogonal to the spray direction when the testing chamber is viewed from above. However, when using the
plate and products other than those specified above, the angle of the main surface with respect to vertical line
shall be as per consultation with the persons concerned.
(2) There shall be no interference with the free fall of the spray.
(3) Solutions collected on one sample shall not drip on other samples.
(4) As a rule, different materials shall not be tested in the same testing chamber at the same time. (However, it may
be conducted as a reference to make comparisons.)
The tests involving salt solution immersion (Method V) shall satisfy the following conditions:
(1) The samples main face shall be placed vertically.

Normative References: NES M 0007-2009 Testing Method for Automotive Paint


JIS Z 2371-2000 Methods of salt spray testing
NES M 0140-2009 Salt Spray Testing

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M0158 [2009-N]
2.3.5 Post-treatment of test samples
After completion of the test, the sample shall be taken out without damaging the exposed surface,
then washed quickly to remove any salt from the surface, and immediately dried at ambient
temperature without removing corrosion. In order to observe surface corrosion, rust shall be removed
by sand blasting or rust removing agent listed in the JIS Z 2371 attachment.

3. TESTING EQUIPMENT
As a rule, the testing equipment shall have the ability to generate and automatically repeat 3 different
processes, i.e. salt solution spraying or immersion, drying and moistening. Depending on the agreement
of parties involved, the test may be performed simultaneously using multiple pieces of testing equipment.
In addition to the above conditions, the testing equipment shall satisfy the following:
(1) Materials used for the equipment shall not corrode under the testing conditions.
(2) The compressed air of the equipment shall not be contaminated with oil and/or dust.
The test involving salt spraying shall satisfy the following conditions:
(1) The spraying nozzle of the test solution shall be set so that the spray does not directly hit the test
sample. Condensed liquid on the ceiling or cover of the testing chamber shall not drip onto the test
sample.
(2) Testing solution used on test samples shall not be returned to the tank and reused.
Examples of equipment are shown in Attachment Figures 1 and 2.

4. TESTING CONDITIONS
Table 1 Compound corrosion test conditions

Name of
Processes in one cycle Cycle conditions
test method

Salt spraying Drying Moistening

60±2°C The atmosphere in the chamber must


<30% RH be “instant setting” with a transition
CCT-I
time of less than 30 minutes, and 1
cycle should take 8 hours.

Salt spraying Drying Moistening


The atmosphere in the chamber must
60±2°C 60±2°C be “instant setting” with a transition
<30% RH 95±5% RH
155 Min 75 Min time of less than 30 minutes. However
CCT-IV 60±2°C 60±2°C Moistening → Salt Spraying process
<30% RH 95±5% RH shall be “conditioned setting” (within
160 Min 80 Min Moistening 10 minutes). 1 cycle shall take less
Drying
Repeat 5 times than 24 hours and 10 minutes.

Salt immersion Drying Moistening The atmosphere in the chamber must


80±2°C 60±2°C be “instant setting” with a transition
<30% RH 95±5% RH time of less than 10 seconds, and 1
CCT-V
55 Min 60 Min cycle should take 2 hours. However,
the process of Drying → Moistening
should take less than 30 minutes.

Note: Instant setting ··········· The time it takes for 1 cycle is fixed, and the time count is started even if the atmosphere has not reached
the stipulated condition.
Conditioned setting ··· The cycle does not proceed to the next step until the atmosphere reaches the required conditions.
Consequently, the time taken for 1 cycle is different depending on the apparatus etc.

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M0158 [2009-N]
Table 2 Applications of each testing method
Application Examples
Corrosion resistance in general (surface rust and penetrated rust): Vehicle body panel, road wheel,
CCT-I
under-floor piping, drive shaft, propeller shaft, fastening parts (bolts and nuts) etc.
CCT-IV External panel scab rust: External panel, external topcoat
CCT-V Internally accelerated penetration of rust: Internal panel, box structure parts

4.1 Salt solution for the test


The salt solution used for salt solution spraying and immersion test and its control method are in
compliance with Items 3 and 4 in NES M 0140.
15 cm
15 cm

15 cm interval
4.2 Salt water spraying condition
Salt water spraying condition and control method are in
compliance with NES M 0140. The control method of
spraying volume that is especially important is excerpted.
As indicated in Figure 1, using any collecting container
within 15 cm interval inside a test chamber, the amount Sampling
of test solution accumulated in the collecting container is container
inspected after the continuous operation for 24 hours or 15 cm interval
more. The amount shall be within the range of specified
2
value (1.5±0.5 mℓ/8.0 cm /h). Do not perform any tests Figure 1 Salt water sampling positions
for the portions that cannot be contained in the range of inside a test chamber
the specified value. If the range that can be within the specified value is small, (1) adjust position and
angle of a nozzle, (2) adjust spraying pressure, and (3) adjust spraying rate by replacing a nozzle, etc.

4.3 Regarding rotation of the test piece during the test (Methods I and IV) containing salt water
spraying
The environmental variations (variations in salt spraying rate, temperature and humidity) within the
tolerance of the specified value for a test condition are due to the difference in installation position for
test piece. Therefore, as a measure for reducing such variations, the rotation of test piece is required.
However, regarding the rotation method and its frequency, they shall be determined through the
consultation between the concerned parties, after considering the required accuracy for the test.
<Case 1> For the test period of 2 weeks or more
Move the test piece any number of times (recommended to perform in the frequency of once per week or more) during
the test period, by an installed unit or by a unit of installed row. For example, if there are 4 installed units, number them
1 to 4 beforehand, and perform the moving of the installed units in the order of: 1→2→3→4→1→ on a weekly basis.
<Case 2> For the test period of 2 weeks or less
Since the number of rotations will be smaller, perform the test within the range of the median value 1.5±0.1 mℓ/8.0
2 2
cm /h (specified value: 1.5±0.5 mℓ/8.0 cm /h) for the spraying rate specified in 16. Spraying rate of the Attachment
Table 1.
<Case 3> For securing the accuracy by long-term test
For the purpose of improving the test accuracy, the following describes the examples of the procedure for complete
randomization of the rotation order:
(1) Number nonnegative integers 1 to n for each test piece number n.
(2) Generate random numbers of nonnegative integers 1 to n for the n installation positions for test pieces.
(3) Install test pieces to each position, according to the numbers that are identical with the installation position numbers
for test pieces.
(4) Perform the rotation of the test piece by repeating (2) and (3) described above any number of times (recommended
to perform in the frequency of once per week or more) during the test period.
0.16
Fluctuation coefficient for the decrease in plate thickness

0.14

0.12
(Standard deviation/mean)

0.1

0.08

0.06

0.04

0.02

0
0 2 4 6 8 10 12
(None) (On a weekly (Once every (On a daily
basis) 3 days) basis)
Number of rotations
2
Figure 1 Rotation effects of SP600 (Standard zinc marking volume at 120 g/m , no chromates)

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M0158 [2009-N]
4.4 Conditions for salt solution immersion
2+
The salt solution for immersion test shall be replaced with fresh solution when the Fe concentration
2+
reaches more than 15 ppm. The Fe concentration shall be determined by methods such as atomic
absorption or inductive coupled plasma spectrometry.

4.5 Maintenance of salt solution for CCT-V method


2+
As shown in the Figure 3, the degree of corrosion changes depending on the Fe concentration in the
salt solution. Therefore, the solution must be changed as required. With metal like aluminum, the
conditions for exchanging the solution shall be added to this standard procedure when the proper
solution concentration is determined.
Decrease in panel thickness (g)

Fe ion concentration (ppm)

(Figure 3) Distribution of observed values at each Fe ion concentration

5. EVALUATION OF RESULTS
The test results shall be evaluated according to relevant material or product standards, or otherwise, the
agreement between the parties concerned shall apply.

6. RECORDING AND REPORTING OF THE RESULTS


The following items shall be reported as test results.
(1) Sample ···· Name, materials and surface coating, shape, dimension etc.
(2) Specification of the testing apparatus
(3) Testing conditions ···· Environment inside the chamber (temperature-humidity charts), number of
cycles repeated, pH of the salt solution etc.
(4) All test results

7. BACKGROUND OF CHOOSING TESTING METHOD

7.1 Choosing test conditions for CCT-IV method

A) Basis for choosing testing method (for coated external part)


The conditions were chosen on the basis of the following premises.
(1) Using exposure results obtained in Okinawa, to maximize acceleration of corrosion.
(2) Use of the 3 step cycle test, i.e. salt spraying, drying and moistening.
(3) Reduce the number of the cycle processes to a minimum, i.e. salt spraying and moistening in one
cycle.
Preliminary investigation conducted varied the exposure time ratio; for drying within the range of 35 to
75%, for moistening within the range of 24 to 66.3% and for salt spraying within the range of 0.7 to 1.1%,
and changing humidity of the moistening step within the range of 80 to 100% RH, respectively.

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M0158 [2009-N]
The results obtained from this investigation to determine the ratios were for drying (66.3%), moistening
(3.3%) and salt spraying (7%), respectively. Because rust streaks appeared with slow acceleration rate
at low humidity, the humidity for the moistening step was chosen to be 95% RH. It was discovered that
the ratio of spray solution is only 0.7% for the whole cycle, and so the solution is sprayed once a day,
considering the accuracy for the spraying volume.
B) Reproducibility in the market (exposure in Okinawa) and acceleration method of CCT-IV method
Figure 4 shows the highly positive correlation between CCT-IV Method and outdoor exposure in
Okinawa using steel panel plated in different ways. Figure 5 compares the acceleration rate of each
test showing CCT-IV Method has an acceleration rate 3 times higher than the current CCT-II Method.

(Reference)
Cycle condition for CCT-II method is described as follows:
Salt spraying (35°C, 2h) → Drying (60°C, 2h) → Moistening (50°C,
95% RH, 4h)
Figure 4 Correlation between CCT-IV Figure 5 Comparison of acceleration rate
Method and exposure in Okinawa for each test method

7.2 Choosing test conditions for CCT-V method


A) Basis for choosing testing method
In order to make possible the evaluation of the panel joint samples and cut-outs from products, salt
solution immersion process was chosen to reduce the otherwise random effects of contact with saline.
Considering temperature, time and the number of cycles to be the most important factors to
accelerate corrosion, these optimal conditions were determined. Sufficient time to completely dry
hemming was referred, consequently the time was varied to adjust for samples’ shape difference.
B) Comparison with other testing methods
The correlation between other testing methods and exposure in Okinawa is given in Figure 6.
The correlation between the new method and market conditions are high for plated steel panels.

Table 3 Correlation coefficient with exposure in


Maximum reduction of the thickness (mm)

Okinawa
Corrosion resistance
CCT-V CCT-III
in salt solution
0.89 0.20 0.60

(Reference)
(note) W2: Durasteel - 1 Cycle condition for CCT-III method is described as follows:
SZ: Durasteel - 2
ZM: Steel sheet and strip
Salt immersion (40°C, 7.5 min) → Moistening (40°C, 95% RH, 15
coated with zincrich min) → Drying (60°C, 7.5 min)
primer for automobiles

CCT-V Exposure in CCT-III Corrosion resistance in salt solution


Okinawa

Reference Diagram 3 Comparison with other testing methods

Figure 6 Comparison with other testing methods

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M0158 [2009-N]
Attachment Figure 1 Compound corrosion test apparatus (CCT-I, II, IV)

Vent

Vent of circulating air


Mixing fan motor

Nebulizer
Mixing fan
Temperature
recorder Dry air supply

Cycle
controller

Control panel

Spray
collection vessel

Testing chamber

Sample piece

Sample piece support

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M0158 [2009-N]
Attachment Figure 2 Compound corrosion test equipment (for salt solution immersion test) (CCT-V)

(1) (2) (3) (4) (5) (6) (7)

(19)

(17)

(15)
(8)
(16)

(14)

(18)

(10) (9)
(13) (12)
(11)

(1) Hydrated specific foam seal (11) Immersion chamber


(2) Upper lid (12) Lift (Cyclic stroke)
(3) Diaphragm (13) Corrosion fluid circulating pump
(4) Sample support (14) Air supplying machine
(5) Dumper (15) Humidity control heater
(6) Air chamber (16) Foaming nozzle
(7) Control panel (17) Humidity controller
(8) Hot air heater (18) Solution cooking apparatus
(9) Heater (19) Exhaust duct
(10) Wind fan

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M0158 [2009-N]
ANNEX
Revision objectives
The evaluation frequency of compound corrosion test in which corrosion of vehicle is reproduced and promoted on
the bench is getting higher. Because this test method was not standardized in the past, there were differences, etc
in test procedures and discrepancies in the test results between parts suppliers and material suppliers.
In addition, conditions which are impossible due to the capability of the tester were specified in conventional test
method.
Accordingly, the test method which has broad utility and is appropriate to the actual condition has been newly
established this time.

Points
(1) Clarification of test conditions
- The transition time to the ambient temperature in each chamber and the teaching method for the tester have
been specified.
- As a rule, the tester obtained from Materials Engineering Department at NTC shall be used as test conditions.
Temperature and humidity charts in the chamber and standard plate thickness reduction at that time are
scheduled to be presented as calibration sample for each tester in the future.
(2) Elimination of Method CCT-II
Though it was developed to evaluate outer body panel coating, it has been eliminated because scab rust on
outer body panel is currently evaluated using Method CCT-IV.
(3) Elimination of Method CCT-III
In the past, it was used for evaluation of parts which are exposed under wet conditions (bottom of the door,
hemmed inner surface, etc.). Recently, Method CCT-I or IV has better reproducibility. Also, it has been
eliminated because time in which the conditions are achieved is very short during 1 cycle of 30 min.

[Revised contents of fiscal 2009]

The following descriptions of procedures related to the test accuracy have been changed and corrected to meet the
actual condition.

1. Descriptions of "2.3.4 Maintaining sample position":


1) Regarding the method for placing sample, descriptions have been changed based on the wording in JIS Z2371,
and descriptions have been added for the case in which parts other than the specified test plate are used.
2) It has been added stating that the test using different materials in the same test chamber is essentially prohibited
in Methods CCT-I and IV.
The background and reason are shown below.
(1) In recent years, the evaluation by mixing with iron test sample in the same chamber is remarkably increased
because the evaluations of light metal materials such as Al and Mg, etc are increased due to weight reduction
in order to reduce the amount of CO2 emissions and improve fuel economy.
(2) Then, there were some cases in which corrosion was unusually promoted or there were significant variations in
performance when using the same test sample because the corrosion powder of iron test sample caused by
the blower during the drying cycle of compound corrosion test adhered to the surface of light metal material test
sample.
However, concrete and quantitative ascertainment that prevent the above phenomenon is insufficient at present.
Specific descriptions into which test accuracy, efficiency and feasibility based on the ascertainment results have
been taken into consideration is an issue in the future.

2. Descriptions of "4.2 Salt water spraying condition" and "4.3 Regarding rotation of the test piece during the test
(Methods I and IV) containing salt water spraying": Descriptions of the amount of salt water to be sprayed have been
corrected.

[Revised contents of fiscal 2004]

As corrosion test results vary greatly depending on the test conditions such as the amount of salt water to be sprayed,
the corrosion tester has been strictly maintained. However, it has been found that the amount of salt water to be sprayed
may not be able to be met in a partial area of the tester due to age deterioration, etc. This time, a stricter control method
of the amount of salt water to be sprayed in the test chamber has been adopted to reduce variations of test results, and
descriptions regarding the rotation of the test piece during the test which is required to be highly accurate have been
added.

1. Clarification of control method of amount of salt water to be sprayed


NES M 0140 is revised and the control method conforms to the contents.

2. Descriptions regarding rotation of test piece


They are included in Item 4.3.

3. Addition of explanation in figure (Addition of reference descriptions regarding conditions of Methods CCT-II and III)

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M0158 [2009-N]
[Revised contents of fiscal 1996]

Because overseas operations reported that humidity was less than 20% under dry conditions during the test using a local
tester, a study has been made as to whether or not adoption should be made. As a result, the humidity conditions have
been revised because humidity of 35% or less has no effects on corrosion under dry conditions. Similarly, it has been
confirmed that there are testers in which humidity is less than 20% also in Japan.

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