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thesis entitled

A STUDY Lb“ 1.11“) CL‘Mn'CiSiCT‘J (5F
z’aU'l‘CMTTBlLL SE‘IEEJT STEEL

presented In]

LeRoy Leonard Peterson

has been 301?]:th towards fulfillment

of the reqltirellwxlts tnr

Lawns— deqrct‘ in Mr .

 

Majul‘ ltrnhtsxur

Date May 19, 19,49

 

 

 

 

 

 

A STUDY OF THE CORROSION OF AUTOMOBILE SHEET STEEL

By

LeRoy Leonardgggterson

- A THESIS
Submitted to the School of Gradnate Studies of Michigan
State College of Agriculture and Applied Science
in partial fulfillment of the requirements

for the degree of

MASTER OF SCIENCE

Department of Chemical Engineering

1949

 

[THESE

 

 

g3

FOREWORD

In presenting this information, it is not the intention of the
author to attempt to fix the responsibility for the corrosion of auto-
mobile bodies on either the manufacturers of motor vehicles, nor on the
governmental agencies using chloride'salts on streets and highways.

.It is felt, however, that this prOblem can best be solved by the
c00perative action of all the organizations connected with.motor
transportation. This information is presented, therefore, not as a
solution to the problem, but as an initial step toward that goal. It
is hoped that this work may, in a small way, contribute to the ultimate
success of their efforts.

The author wishes to thank Dr. C. C. DeWitt, Dr. M. G. Larian,
and Dr. R. W. Ludt of the Chemical Engineering Department for their
helpful counsel and guidance. Sincere appreciation is expressed to
us. E. A. Finney, Mr. C. C. Rhodes, Dr. Richard Thurm, and the other
members of the Michigan State Highway Research Laboratory for the
friendly assistance and cooperation which contributed so much to the
completion of this work. Without their assistance, this project

would not have been possible.

L. L. Peterson
May 19, 1949
East Lansing, Michigan

{21789 8

TABLE OF CONTENTS

Introduction . . . . . . . . . . . . . . . . . 1
Factors Affecting Corrosion . . . . . . . . . . . . 5
Scope and Gen eral Pro ced'ure e o o o o o e o o o o e 5

Inhibitor Study 0 e o o o o o o o o o o o o 5
Study of the Corrosive Media . . . . . . . . . . 7

Discussion of Results_ . . . . . . . . . . . . . . 8
Chromate Inhibitors o o o o o o o o o o o o o 9
Phosphate Inhibitors o o o e o o e e o o o e o 18
Corro Sive Media. 0 o o o o e o o o e o o o o 25

COHCIUSions o o o o e o o o o o o o o o o o o 51

Appendix A o o o o o o o o o o o o o o o o o o 55

Data Sumry (Tables 1-12) 0 o o o o o o o o o o 54
Plate PhOtographs (Figures 15"18) o e o o o o o o 46

Appendix B o e e o o o o o o o o o o o o e o o 74

Laboratory Procedure . . . . . . . . . . . . . 75
Equations 0 e e o o o o o o o o o o o o e 80
Brine Analyses . . . . . . . . . . . . 81
Chloride Content Of Road.81u5h. o o o o o o o e o 82
T9813 Plate Measurement 0 e o o o o o o o o o o 85
original Data to o o e o o o o o e o o o o o 8 5
Selected References . . . . . . . . . . . . . llO
Supplementary Biblio graplw o o o o o o e o o o o 112

A STUDY OF THE CORROSION OF AUTOMOBILE SHEET STEEL

In recent years, the problem of automobile body corrosion has
become increasingly troublesome to motorists. The extensive use of
the automdbile as a means of transportation has demanded that streets
and highways be kept safely passable under all weather conditions. To
this end, sodium chloride and calcium chloride have been applied as
a means of ice control and dust palliation. The use of these chemicals
has mounted in direct proportion to the increasing traffic on our highe
ways and has brought the prOblem of corrosion sharply to the attention
of the motorist. The opinion of a great majority of motorists seems
to be that these chloride salts are the chief cause of this destruc-
tion (Figure 1).

Little published information is available on this specific phase
of chloride salt corrosion, although some work on this prdblem has
.been reported in recent periodicals and press releases. These reports
have apparently been based on opinion and visual field surveys, lacking

(1) (2) (5) (16)
in quantitative support. . However, considerable data may be
feund on the corrosive properties of refrigerating brines and sea
waterSS) Speller(7)gives an excellent bibliography on the general
subject of corrosion.

This investigation concerns the feasibility of reducing the
corrosion of automobile bodies by the addition of corrosion inhibitors
to the chloride salts used on streets and highways. Since a thorough
study of the complete problem of automobile body corrosion would
require a very extensive investigation, the scope of this work has

been limited to a laboratory study of the corrosiveness of sodium

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and calcium chloride salts and of the effects of various corrosion
inhibitors.

FACTORS AFFECTING 0012303191

Generally, corrosive action is similar to the action occurring
in a galvanic cell. Just as the galvanic cell has positive and
negative terminals, so a sheet of metal has positive and negative
areas. There may be a great many of these oppositely charged areas
on a single sheet of metal. These areas are caused by internal
stresses, heterogeneity, ruptures in a protective coating, and many
other factors. Corrosion takes place when metal dissolves at the
positive area, or anode. The corrosion products are generally depos-
ited on the negative area, or cathodef7)(8) These corrosion products
form a film over the negative region, isolating the metal and thus
retarding corrosion. Excellent examples of the formation of very
thin, dense and adherent films of corrosion products over the metal
surfaces are afforded by stainless steel, chromium, and aluminums

Corrosion continues when this film is mechanically or chemically
broken. In the case of chromium, aluminum, or stainless steel, film
destruction is very difficult. Other metals, such.as iron and steel,
form.filme of corrosion products which are easily removed or broken,
thus allowing corrosion to continue. Many agents such.as oxygen,
abrasive action, or the presence of certain chemicals accelerate the
breakdown of the film of corrosion products.

It is the function of corrosion inhibitors to form new or repair
the old films on the surface of the metalsg) Inhibitors are classified
as anodic or cathodic depending on whether they form a film.over the
positive or negative areas of the metal. The isolation of the metal

-5-

from the corroding medium is essential if corrosion is to be pre-

vented.

Consideration of the prdblem of automobile body corrosion indi-

cates that the following factors are involved.

1.

2.

5.

4.

5.

6.

7.

8.

A.corrosive brine is formed as a result of the use of
sodium and calcium chlorides on roads for dust palliation
and ice control.

Rain and other forms of precipitation, in the absence of
chloride salts, cause corrosion.

In industrial areas sulfur dioxide-laden rain and moisture
contribute to active corrosion.

In the case of rock salt, crystal growth.by evaporation
may mechanically loosen the protective paint coating.
Calcium chloride leads to corrosion by holding moisture

in cracks and crevices.

.Accumulation of water, with.or without dissolved chloride
salts, in hollow body members such as doors, door posts,
and running boards likewise contributes to the corrosion
picture.

Abrasive action of sand and pebbles thrown against the
body breaks paint coatings and films of corrosion products.
Soil and other foreign matter, comprising the mud that
exists underneath an automObile, materially affects the

character of the corrosion.

‘The changes in metal thickness and the stresses set up in

the metal by deep-drawing Operations contribute largely

to localized corrosion failures.

-4-

The above factors Will, directly or indirectly, affect either
the actual dissolving of the automobile steel and the continual des-
truction of the protective film of corrosion products. In this paper,

only the first of these factors will be considered.

CO G

The investigation was divided into two major parts. First, an
examination of several inhibitors was undertaken. This was done to
determine which inhibitors might be effective in reducing the corro-
siveness of the chloride salts. The second part of the investigation
consisted of a comparison of the corrosive effects of distilled water,
sodium chloride, and calcium chloride. Its purpose was to learn whe-
ther or not the chloride salts were more corrosive than rain or
ground water.

Throughout the investigation, the chloride concentrations are
given in weight-per cent based on the weight of water in solution.
The inhibitor (or inhibitor mixture) concentrations are in weight—
per cent based on the weight of total chloride salts in solution.
The various components of the inhibitor mixtures are given in parts
by weight, with.the entire mixture taken as 100 parts. In all cases,
except-the elimination study, triplicate samples were tested.

bi ‘ St

In studying the effects of the various inhibitors, eleven series
of tests were conducted. The test periods were two weeks initially,
but were increased to four weeks later on. Room temperature (75° F.’
was maintained throughout the inhibitor tests.

-5-

Series 1 was an elimination test of several inhibitors and
inhibitor mixtures conducted on single samples. The inhibitors were
used in concentrations of 0.5 per cent. The corrosive solution was a
5 per cent calcium chloride brine, saturated with oxygen by a con-
tinuous flow of air bubbles.

Series 2, 5, 6, 10, 11, and 12 were confined to a study of
chromate inhibitors. Samples were continuously aerated throughout the
test. In series 2 the effect of various organic additives on the
inhibitive efficiency of sodium chromate in a 5 per cent calcium
chloride brine was studied. Series 5 compared the inhibitive prop—
erties of sodium chromate and sodium dichromate at various concen-
trations in a 5 per cent rock salt (NaCl) brine. The effects of
hydroquinone on sodium dichromate and of quinone and quinhydrone on
sodium chromate in a 5 per cent calcium.chloride brine were examined
in series 10. In series 6 the Optimum sodium chromate-hydroquinone
ratio was determined.by varying the proportions ofeach at a constant
concentration of inhibitor mixture. This was done in a 5 per cent
and a 20 per cent calcium chloride solution. An effert to ascertain
the minimum effective inhibitor concentration was made in series 11,
by using various concentrations of a fixed sodium.chromate—hydroqui-
none mixture in a 5 per cent calcium chloride brine. Series 12 was
identical to series 11, except that sodium chromate alone was used.

In series 4 the effect of road soilcnzinhibition efficiency was
studied. ‘A mud consisting of road soil passing a 50-mesh sieve and
{a saturated calcium chloride brine was made up to simulate a graveled

road immediately after a chloride application. Weighed metal plates

-5-

were immersed in the mud for eight hours and exposed to the air for
sixteen hours over a period of twentyaeight days. The plates were
cleaned and weighed once each week according to the procedure des-
cribed in Appendix.B, and returned to the test. This was done at
room temperature with.brines containing varying amounts of sodium
chromate as an inhibitor.

In series 7 several phosphate inhibitors were tested at a l per
cent concentration in a 5 per cent calcium chloride brine and a 5 per
cent rock salt (NaCl) brine. The metal plates were alternately im-
mersed in the brine and exposed to the air. This test was repeated
in series 8, except that the metal plates were continuously immersed
in aerated brines. These two tests were performed in order to compare
> the continuous aeration and alternate immersion types of tests. In
series 9 several other phosphate inhibitors were tested at 0.5 per
cent concentrations in both.a 5 per cent rock salt brine and a 5
per cent calcium chloride brine.

Study 9; the Corrgsive Media

In this study, the influence of temperature, aeration, and
agitation on the corrosive effects of distilled water, sodium chloride,
and calcium chloride was investigated. Brines of various concentra-
tions were used, ranging from distilled water to a saturated brine for
both calcium chloride and rock salt.

Series 5, l4, and 15 were all continuously aerated tests. Series
5 and 15 were run at 75° F. and were identical, except that series 15
included rock salt solutions. Series 14 was the same as series 15,

except that it was conducted at a temperature of 55° F.

-7-

Series 15 and 16 were conducted under conditions of limited ac-
cess to air by placing the specimens in sealed jars. The brines were
prepared with distilled water that had been freshly boiled. The two
tests were the same, except that series 15 was conducted at 55° F.,
while series 14 was run at 75° F.

The detailed procedure for all of these tests may be found in
pp. 75-79 of Appendix:B. Series 1, 2, 5, 5, 6, 8, 9, 10, ll, 12, 14,
and 15 were conducted according to cycle 1; series 7 according to cycle
2; and series 15 and 16 according to cycle 5. Series 4 was performed as
previously stated. Data summaries and photographs are located in pp.
55-75 of Appendix A. All original data is included in pp. 85-109 of
.Appendix B.

DISCUSSION OF RESULTS

The chief factors affecting the results of all these tests seemed
to be temperature and aeration. The temperature variations were within
: 5° F. and did not appear to introduce any appreciable errors. The
control of aeration, however, was not completely satisfactory.

.According to Speller(7)the supply of oxygen to the metal surface
is influenced.by the solubility of oxygen in the solution, the physical
distribution of oxygen throughout the solution, and the rate of diffur
sion of oxygen across the liquid film at the metal-liquid interface.
Since the degree of aeration affects all of these factors, and since
oxygen is essential for ordinary cases of corrosion, it can easily be
seen that aeration is a critical factor. In concentrated brines and
in the presence of an effective inhibitor, i.e. at low rates of corro-

sion, no appreciable variations were noticed. However, in dilute

brines, i.e. at high rates of corrosion considerable uncertainty was
-8-

observed. At these high corrosion rates, the supply of oxygen to the
metal was apparently the controlling factor, rather than the nature cf
the solution itself.(10)

Although it is well recognized that pH and its proper control
exert considerable influence on corrosion, it was deemed unnecessary
to control pH in these tests. The reason for this decision was the
apparent impracticability of controlling pH over miles of road surface
under widely varied conditions. For this reason, it was decided that
an inhibitor should be effective without any particular attempt at pH
regulation.

The pH of some of the solutions was, however, checked with a
Beckman pH meter at intervals throughout the tests, pp. 87-109,
Appendix B. The only significant trend noticed was a general decrease
in pH as corrosion progressed. The higher rates of corrosion also
appeared to be accompanied by a larger pH drop for aerated solutions.
The unaerated tests, however, sometimes exhibited an increase in pH.

All data presented represent the average results of three samples.
Chromate Inhibitorg

The data of Table 1 and Figure 2 show that the corrosiveness of
a 5 per cent sodium chloride brine was reduced considerably for a
period of fourteen days by either sodium chromate or sodium dichro-
mate. There appeared to be very little difference in the behavior
of the two, although the chromate lost most of its effectiveness at
low concentrations after about seven days.

In series 4 an attempt was made to determine what effect soil
particles would have on the effectiveness of inhibitors. This
attempt was unsuccessful because the brine used was too highly

*9“

concentrated to show any significant trend (Table 2). A later analysis
of road slush showed that the actual concentration of chloride salts
present did not exceed 2 per cent, pp. 82, Appendix B. This confirms
the data reported. by Finney.(15)

From Figure 5 and Table 5, it can be seen that sodium chromate
alone was fairly effective in reducing the corrosiveness of a 5 per
cent calcium chloride brine, losing its effectiveness after about
fourteen days. The addition of small amounts of pyridine, sodium sali-
cylate, formaldehyde, or sodium benzoate increased the effectiveness of
the inhibitor only slightly. However, the addition of hydroquinone
maintained the effectiveness for at least 21 days.

The effect of quinone, hydroquinone, and quinhydrone on sodium
chromate as an inhibitor is shown in Table 4 and Figure 4. They all
appear to affect the inhibitive properties of sodium chromate in about
the same manner. This would be expected in view of their chemical
similarity. Sodium dichromate behaves in the same way in the presence
of hydroquinone as does sodium chromate.

xAn examination of Table 5 and Figure 5 reveals that, for a 5 per
cent calcium chloride brine, increasing the hydroquinone-sodium chro—
mate ratio resulted in a sharp drop in the corrosion rate down to a
minimum, after which there was a comparatively gradual increase. The
total concentration of inhibitor mixture was held at 0.5 per cent
throughout the test. The optimum proportions of sodium chromate and
hydroquinone appeared to be in the range of 80 per cent chromate-20
per cent hydroquinone to 90 per cent chromate—10 per cent hydroquinone.
However, for a.20 per cent calcium chloride brine, there appeared to
.be little advantage to the use of hydroquinone with sodium chromate.

-10..

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~15-

In series 11 and 12 it was desired to learn at what concentration
the sodium chromate was most effective, and what influence the addition
Of hydroquinone exerted on this concentration. Tables 6, 7, and Figure 6
show the minimum effective concentration to be about 1.5 per cent of the
weight of the total chloride salts in solution, whether or not hydroqui-
none was present. In fact, the curves indicate that the presence of
small amounts of hydroquinone has practically no effect on the inhibitive
properties of sodium chromate. Although these results were not in agree-
ment with thoseof Figures 4, 5, and 6 time limitations did not permit
a duplication of the tests.

In spite Of the lack Of agreement with the previous data, some
interesting information can be obtained from series 11 and 12. An
examination Of Figures 15 and 14 reveals that at low inhibitor concen-
trations, the corrosion appears to be rather evenly distributed over
the surface of the metal as evidenced by the even coating of light
red rust. IAs the inhibitor concentration is increased, the appearance
Of large uncorroded areas can be noticed, accompanied by rather hard,
dark red blisters over the corroded regions. This type Of corrosion is
known as pitting corrosion.

It can also be noticed that areas which were once pitted and then
cleaned during the weekly cleaning and weighing were not necessarily
sUbJect to continued attack on being reimmersed in solution. 0n the
contrary these areas often appear to be completely protected. This
can probably be explained on the basis Of a change in polarity of the
pitted areas. It is now widely accepted that rust ordinarily forms by
electrochemical loss Of metal at an anodic region, the corrosion
products being deposited at the cathode.(ll) For this reason, it would

-15-

seem that the once-pitted areas had, after cleaning, becomeccathodic
relative tO certain other areas on the metal surface.

It will also be noted that pitting appeared at about the same
inhibitor concentration, see Figure 6, at which the corrosion rate
became relatively constant.' In the light of this fact and the pitting
exhibited by the photographs, it can be seen that althOugh the rate of
corrosion has decreased, the area actually subjected to corrosion has
decreased also. This indicates that the corrosion taking place under
the blisters is probably more rapid than the data lead one to believeElZ)
This indicates that the metal may actually corrode completely through
I in a much shorter time over a small area under pitting conditions than
under conditions Of overall corrosion.(9) According to Hoar and Evansflz)
pitting diminishes and finally ceases as the chromate concentration
increases.

IAlthough some of the preceding data regarding hydroquinone as an
additive to sodium chromate are contradictory, there is a strong indi-
cation that hydroquinone may have some beneficial effect. ‘The opinion
of some authors is that the chromates could not be expected to main-
tain their effectiveness as inhibitors in the presence of easily
oxidized material.(l4)(15) It would seem that these statements were
based on the fact that the chromates, being oxidizing agents, would
be reduced in the presence of easily oxidizable material. The
results of these tests show, however, that the chromates maintained
their effectiveness whether or not hydroquinone was present. Moreover,
the effectiveness of the chromates was, in some cases, actually

increased.

-17-

IAcceptance of the fact that the chromates would be reduced by
easily oxidizable material, such as hydroquinone, merely leads to
speculation as to the effect Of chromous ion as a corrosion inhibitor.

Generally, these data show that there may be some merit to the
addition Of hydroquinone to sodium chromate for corrosion inhibition,
although this is not conclusive. Pitting conditions persist at
chromate concentrations of 5 per cent Of the weight of dissolved
chloride salts, even though the data indicates marked leveling Off
in corrosion rate at about 1.5 per cent.

Phpgphate Inhibitors

In studying the phosphate inhibitors, the tests were performed
with.a twofold purpose: First, to evaluate certain commercial glassy
sodium phosphates for use in reducing the corrosiveness of sodium
chloride and calcium chloride brines. Second, to compare the aerated
method of test to the alternate immersion method being used by some
phosphate manufacturers. Three proprietary products were studied
primarily and used as a guide in evaluating the other phosphates.
These products may be identified as follows:

1. - Micromet - A slightly soluble complex sodium-calcium
hexametaphosphate used for rust prevention in household
water systems.

2. - Calgon - Sodium hexametaphosphate, containing about 67
per cent P205, used extensively for feed water treatment.

5. - Banox - Reported to be a mixture of Calgon and calcium

chloride, it is used as a corrosion inhibitor for surface

treatment of steel prior to painting and for addition to

-18-

 

 

 

 

 

 

 

 

 

 

 

 

 

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/.*
7
T I M E

AERATION a AGITATION AT 75°F
SERIES NO.8

 

 

 

 

 

 

 

 

EFFECT a/ GLASSY PHOSPHATES ad
CORROSION INHIBITORS [,2 5% C.CI -M,CI BRINE

Io GAUGE SAE ‘IOOS SHEET STEEI.

\

Figure 7

-19-

I 600

 

 

 

 

 

 
   
 
 
 

 

 

 

 

 

 

I400 %
:2 /
\ L E G E N D W I AL
{I200 N0 INHIBITOR / I
" —-— I‘lo MICROMET ll
——-- Iv. GALGON /’
z
—-— l'/ BANOx ,
° . L / ’ j
- IOOO I; .-
o'I / I /
o , /
I
3 Z J’
’ U
“ BOO ______ 1
O // I /
U I ’ i .

 

I
’ 0
fl ” /
I
600 F— ’,

 

 

 

CUMULATIVE

 

 

 

 

 

 

 

 

2| 26

AERATION a. AGITATION AT 75°F
SERIES No.8

EFFECT a/ GLASSY FHOSPHATES M
CORROSION INHIBITORS [,2 5% C.CI -M,CI BRINE

Is GAUGE SAE ‘Iooe SHEET STEEL

¥

Figure 7

-19-

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

100
- coo
a LEGEND
\
9 N0 INHIBITOR

------- w. GALGON

z —-—w. MIGROMET
O
” 400
O
C
K
O
U

300
In]
>
g...
< 200
J
D
x
a
U

I00

.I'
l
o "'"l 7
0 7 I4 2' 28
T I M E ‘ o A Y s )

SERIES NO. 7

 

 

BFFBCTufGLASSY FHOSFHATES as
CORROSION INHIBITORS m 5% CaCIz- M,CIZBRINE

ALTERNATE IMMERSION AT M, I9 GAUGE SAE'IOOO SIEET STEEL

-
I

Figure 8

-20-

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

SERIES No.8

 

 

EFFECT 47/ GLASSY FHOSPHATES ad
CORROSION INHIBITORS 02 5% ROCK SALT BRINE

IO GAUGE SAE'IOOO SHEET S

 

Figure 9

-21..

 

700

 

 

 

 

 

 

 

 

,‘000
" T
x LEGEND
o
\
O NO INHIBITOR >
1 500 --——--I% BANOx /4
- -------- w. CALGON
——~—deaIMGROMET
Z
O
n 400 .
O
C
(I:
O
U

 

300

 

ZOO

 

 

CUMULATIVE

 

IOO

 

 

 

 

 

SERIES NO. 7

EFFECTuf CLASSY FHOSFHATES 44.
CORROSION INHIBITORS m 5% ROCK SALT BRINE

IO GAUGE SAE'IOOO SHEET STEEL,ALTERNATE IMMERSON AT 75"

g
¥

Figure 10
-22-

rock salt for use on highways.

A glance at the data of Tables 8 and 9 and Figures 7 and 8 show
that in concentrations of 1 per centIthe above-mentioned phosphates were
ineffective in reducing the corrosiveness of calcium chloride brine. In
sodium chloride, however, (see Figures 9 and 10) it is evident that the
behavior of Micromet and Banox was about the same as in calcium chloride,
while Calgon stood out as being very effective.

The data Of Table 10 are in general agreement with the preceding
data. HOwever, disodium phosphate and trisodium phosphate were ineffec-
tive in rock salt brine. Nalco 519, a commerical sodium septaphosphate,
deserves mention as being very effective with rock salt.

The behavior of these inhibitors can probably be explained on the
basis that the sodium hexametaphosphate prevalent in these materials
forms a relatively insoluble calcium phosphate complex in calcium
chloride. This would remove a large portion Of inhibitor from solution
by precipitation before a sufficiently protective film could be formed
on the metal surface. In the case of sodium chloride (rock salt) the
basic reason would probably be the same, with.the calcium.ion being
furnished by the inhibitors themselves (Micromet and Banox) on being
dissolved, along with a small amount of calcium ion present in the rock
salt as gypsum. The calcium present in the rock salt was apparently not
sufficient to affect the inhibitive properties Of the plain sodium
hexametaphosphate.

The results of the alternate immersion test, series 7, and the
sierated test, series 8, were in qualitative agreement with each other.

Iiowever, the degree Of corrosion Obtained in the aerated test was much

-25-

higher than in the alternate immersion test. Apparently, then, the
aerated test would be a more rapid means for laboratory evaluation of
the properties of corrosion inhibitors.

From these data it appears that the presence of considerable
amounts of calcium ion relative to the amount of phosphate is undesir-
able when the phosphate inhibitors are used. This is in general agree-
ment with the work Of Hatch and Rice.(15)

These data show that the phosphates are not suitable inhibitors
for calcium chloride salts. However, Calgon and Nalco 519 show promise
of being effective for sodium chloride. The continuously aerated test
seemed to be more severe than the alternate immersiOn test, although
their correlation was fairly good.

All the inhibitors included in this study may be classified as
anodic inhibitors. It is a characteristic of anodic inhibitors that
they sometimes cause the pitting effects shown in Figures 15 and 1459)
This would be especially true at the crevices and corners under an
automObile body where access is difficult. It would, therefore, seem
that use of these inhibitors, particularly in low concentrations
involves a certain amount Of risk.

If these data are plotted to show the cumulative loss in weight
(corrosion) versus time, as in Figures 2, 5, 4, 7, 8, 9, and 10 the
length of time any given inhibitor retains its effectiveness may be
ascertained. As the inhibitor loses its efficiency, the slope Of the
corrosion curve for the inhibited solution becomes steeper, until it

is approximately parallel to the corrosion curve for the same uninhibited

solution. In other words, the rate Of corrosion gradually increases

-24-

until it becomes about the same as that of an uninhibited solution.
W

In series 5, 15, 14, 15, and 16 an attempt was made to shed some
light on the question as to whether solutions of chloride salts were
more or less corrosive than water. This was deemed necessary in view
of the volume of seemingly contradictory data to be found in the
literature. Whitman, Russell, and Davis(l7)show that dilute solutions
Of chloride salts are more corrosive than water, with a gradual de-
crease in corrosion as the chloride salt content is increased. Spell—
er(18)reports Richardson as showing distilled water less corrosive
than a 10 per cent salt brine for six different irons in both the stag-
nant and aerated alternate wetting and drying type tests at room
temperature. Richardson also shows distilled water as being more
corrosive than a 10 per cent salt brine for the same irons in both the
stagnant and.aerated continuous immersion type tests at r00m.temperature.
Friend and Marshall(19)indicate tap water as being only very slightly
less corrosive than a 5 per cent NaCl solution for a three month conti-
nuous immerSion test. Friend<20)later reports tap water as being more
corrosive than a 5 per cent NaCl solution for three different steels in
a one-year continuous immersion test at 50° F. Friend and.Brown(4)
report that at about 15° C. dilute NaCl solutions and distilled water
are about equally corrosive. .At temperatures above 15° C., dilute
solutions of NaCl are more corrosive than distilled water, while at
temperatures below 15° C. dilute NaCl solutions are less corrosive
than distilled water. Corrosion gradually decreases for higher concen-
trations at all temperatures.

.25-

 

I20

 

I00 I '

 

 
 
 
 
 

 

L E G E N D

CaCI, 75"
""" NaCl TSTF
---- NaCl JS'F
- ‘ "' CLCI. 35°F

 

 

 

 

 
   
 

 

(Maldwl DAY)

 

 

 

CORROSION RAT E

 

 

 

 

 

 

 

 

 

O S IO IS
TOTAL CHLORIDE SALT CONCENTRATION (Wt-A) '

CONTINUOUSLY AERATED AND AGITATED
SERIES I4 a I5

 

 

‘
‘

EFFECT u/TEMFERATURE wz t/zE CORROSIVENESS
u/C.Ct_ ans/NaCl BRINES

 
 

R—_‘_ _ _

 
 

 

 

 

 

 

 

 

 

(Mal JM'IOAY)

 

 

 

CORROSION RATE

 

 

 

.‘fi-II

 

 

 

 

 

 

 

 

 

0 5 IO IS 20 as 30
TOTAL CHLORIDE SALT CONCENTRATION (V1170),

STAGNANT, LIMITED ACCESS To AIR
SERIES ISSIO

g

4

EFFECT ufTEMPBRATURE U72 1%; CORROSIVENESS
(yam: and/NaCl BRINES

 

 

 

 

 

 

Figure 12
-27-

The results Of series 5, l5, 14, 15, and 16 given in Tables ll and
12 contain some Of the above-mentioned discrepancies. In these tests
it is believed that the variations were due to difficulty in control of
the rate of aeration. However, the general trends shown in Figures lland
12 are fairly well indicated. The results Of the aerated tests, Figure
11, exhibit the same trends as those Of Whitman, Russell, and Davis,(l7)
and of Friend and.Brown for temperatures below 15° C. However, the
relation between the corrosiveness of dilute salt solutions and water
did not reverse with change in temperature as reported by Friend and
Brown, even though the temperatures used were in the same range. The
results of the unaerated tests, Figure 12, follow the pattern of Friend
and Brown at temperatures above 15° C.

The overall corrosion rate of series 5, Table 11, follows the same
pattern as does Figure 11 for Ca012 at 75° F. However, the weekly
rates show considerable variation for dilute solutions.

The character of the corrosion which took place in series 15, 14,
15, and 16 is illustrated in the photographs Of Figures 15, l6, l7, and
18. There were two distinct layers of corrosion products formed on
the surface of the metal. The outer layer consisted of a hydrated
ferric oxide mixture varying in color from an orange-red for distilled
water and dilute brines to a redébrown fer the more concentrated solu-
tions. The darker colored products seemed to adhere to the metal more
firmly than did the light colored scale.

A.dark blue-black layer of ferrous oxides and hydroxides was
found underneath the outer layer. This dark layer was particularly
noticeable in series 15 and 16 where the air supply was limited, indica-

ting insufficient oxygen to convert the ferrous products to the ferric

-23-

state.

Plates 1a, 1b, 10 of series 14 for distilled water exhibited very
little corrosion as may be seen in Figure 15—1. However, these plates
seemed to have a rather peculiar yellow—green film over the surface at
conclusion of the tests. This film was not present in the other dis-
tilled water tests. For this reason, the results Of plates 1a, lb, and
1c were discarded.and the results of plates 6a, 6b, 6c substituted.

The results of the unaerated series 15 and 16, Figure 12, show
distilled water at 55° F. to be more corrosive than any concentration
of either NaCl or Ca012 at the same temperature. However, at 75° F.
dilute CaClz solutions appear to be more corrosive than distilled water,
while NaCl exhibits the same characteristics as at 55° F. The increase
in corrosion by the dilute CaCl2 over that for distilled water was
about 25 per cent. The corrosion rates shown here appear to follow
very closely the same pattern as the oxygen solubility curves for
solutions Of various salts given by Speller.(21) Increasing the
temperature from 55 to 75° F. did not appear to affect the corrosiveness
Of NaCl appreciably.

Figure 11, series 14 and 15, shows that at 55° F. dilute solutions
Of both.NaCl and Ca012 increase corrosion over that for distilled
water by about 20 per cent. At 75° F. dilute NaCl solutions continue
to be more corrosive than distilled water. However, the behavior of
dilute CaC12 solutions at 75° F. is not understood.

Increasing the temperature from 55 to 75° F. resulted in a
marked increase in corrosion for all but the most concentrated solutions.
At 55° F. no concentration of either CaC12 or NaCl showed as much corro-

sion as did distilled water at 75° F.

.2 9...

Furthermore, it can be seen that the corrosion rates are much higher
at either temperature under conditions of aeration and agitation than
under limited air supply and quiescent conditions. The combined effects
of agitation and air supply produced a corrosion rate from 50 to 80 times
greater than in their absence. Apparently the presence or absence Of
oxygen at the metal surface is Of prime importance in the corrosion
reactions taking place.

Hewever, the mere presence or absence of oxygen does not explain
the results shown in Figure 11. There appear to be several variables
which contribute to the results shown and greatly complicate the
situation. Speller shows that for water with free access to air corro-
sion increases with temperature up to about 175° F. and then decreases
with further increase in temperature.(22) This is eXplainable on the
basis that oxygen solubility decreases as temperature increases. How-
ever, the increase in temperature affects those factors which increase
the transfer of the dissolved oxygen to the metal surface as follows:
(1) The viscosity of the solution decreases, resulting in more effi-
cient distribution of oxygen throughout the liquid. (2) The rate of
diffusion of oxygen across the liquid film at the liquid-metal inter-
face increases, thus carrying the oxygen to the metal faster. (5) The
liquid film at the liquid-metal interface decreases in thickness,'thus
decreasing the time required for diffusion. In addition to these
factors, the c0rrosion reactions take place faster at the higher temp-
eratures provided there is enough Oxygen present to permit the reactions
to take place. It is, therefore, apparent that the corrosion will
increase with increasing temperatures, until the factors tending to

-30...

increase corrosion can no longer compensate for the decrease in oxygen
solubility. Beyond this point corrosion will decrease as Speller has
demonstrated.

It seems that these conditions would also be true for solutions of
salts, with the additional condition that oxygen solubility decreases
with increasing salt concentrations.(22) There should, therefore, be
an inversion temperature similar to that for water in the case Of salt
solutions. However, this temperature may be different for each concen-
tration and type of salt. FUrther work certainly seems to be indicated
on the effect of temperature on oxygen solubility in various concentra-
tions of different salts, and on the corrosiveness Of these salt
solutions.

Generally, these data show that oxygen is of major importance in
the corrosion reactions. Under identical ordinary conditions, dilute
chloride salts were about 20 to 25 per cent more corrosive than dis—

tilled water. However, distilled water at 75° F. was nearly twice as

Corrosive as any chloride salt solution at 55° F.

CONCLUSIONS
Although these results must be interpreted cautiously until
confirmed by tests under field conditions, the following conclusions
may be made:

1. - In order for an inhibitor to be considered satisfactory, it
must reduce corrosion without setting up pitting conditions;
and it must do so at concentrations that are economically
practical for highway usage.

2. - 0f the inhibitors studied, only three appear to merit further

-51-

consideration for use. The chromates should be considered
for use in either sodium or calcium chloride, while Calgon
and Nalco 519 should be considered for use in rock salt only.

NO inhibitor should be used, however, unless it has been

thoroughly tested, since it may actually increase the corrosion

in localized areas by setting up pitting conditions rather

than reducing the damage due to corrosion.

5. - Although there appears to be strong indications that hydro-

50"

quinone, quinone, or quinhydrone may have some beneficial
action on the effectiveness of the chromate inhibitors,

this is not conclusive. Further work on this point is
indicated, including study of the effect of chromous ion as
an inhibitor.

Under the same conditions, chloride salts are generally from
20 to 25 per cent more corrosive than distilled water. Hew—
ever, distilled water is much more corrosive at ordinary
spring and summer temperatures than any solution Of chloride
salts is at ordinary winter temperatures.

Chloride salts probably do not contribute nearly as much to

the corrosion of automObile bodies as is popularly believed.

6. - Although the inhibitors tested may possibly reduce the

corrosiveness of the chloride salts, inhibition of these
salts cannot be justified on the basis of present

information.

-52-

APPENDIX A

2h

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SERIES II

EFFECT OF CHROMATE CONCENTRATION ON

CHARACTER OF CORROSION
5% cat-Mpg BRINE, AERATED & AGITA‘TED AT 75°F
FHURE l3-l
-45-

 

 

 

EFFECT OF CI—Iiv. 37.4. I "ICENTRATION ON

CHARfiI-TiR (“F CORROSION
«25, AERATED a AGITATED AT 75°F

5°/o CACIL‘ v‘I‘I ' _
FI'B’JRE I3-2

..47-

-. __.——_.,.r)_~_

 

 

 

 

 

 

 

 

 

 

 

 

    

. g; . ‘
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l
y;

7’5"“)? f)? 3.21,;-
A .15 ,l . ‘ ‘

   

EFFECT OF CHP‘DMA'I‘E CONCENTRAT|ON ON

CHARACTER OF CORROSION
5°/° C*C'2_‘ M- :‘g 95" Nil, AERATED 3‘ ACETATED AT 75°F
FI'S'JRE I3-3

'48-

”-.. __

 

EFFECT OF rL CONCENTRATiON ON
C¥~:.r.-.~‘1-.;;sf."‘ if? OF CORROSION
5°/o CALI-"Ari; I—sHINE, AERATED & AGITATED AT 75°F
Fz'mRE l3-4
-49-

 

 

 

 

EFFECT OF CHROMATE ~HYDR’QUINONE CONCENTRATION ON
CHARACTER OF CORROSION
5%.» ecu-M10, 691.25., AERA‘I’ED t AGITATED AT 75'?
FIGURE I4-I
-50-

 

 

 

EFFECT OF CHROMATE :w-at,.-.-g.e::--:Oz~ls=. CO:«2CENTRATION ON
CHI‘Mflx-CTE’H O? CORROSION
55°/o CCCIfM‘CI. Emma, AERATED I. AGITATEO AT 75°F
nouns 14-2
. 5|.

 

-\

EFFECT OF CHROMATE m’r%YDHC';’-.'IT‘I:ONE CONCENTRAWON ON

CHARACTER OF CORROSION
5°/o Cng-MICTZ E.“ ‘.;., ACHATED & AGITATED AT 75°F
qupF |4-3
-52-

 

EFFECT OF CHQé’SMATE. HYDROQ . . {-éCI'NE C.O'°:AT§ON ON

CHARACTER CORROSION
' 3O Coca-Evid’fi‘ ;:f.':'.{1r.., AERATED ‘ AGITATED AT 75°F
FIGURE I4'4
-53-

 

 

 

. ¢ . . - A
t ' .‘ I " "' '3
’ ‘r A ° \.\_3

-—°-*'; ..--

CORROSIVE EFFECTS OF HZO,C;C13~-MiClZ
' AND MCI AT 35°F LNOT AERATED)

FIGURE l5-l
-5‘4—

 

 

 

("I.‘fQQQ..IF: FF IF“ FIE-‘3) CLCIL *‘I‘~1’I?CI'_‘.
~ND f . 7 .F J5°F (NOT AERATED)

FIGURE l5-2
-55-

 

-~ um

AT 35°F (NOT AERATED)

A .

I‘VE"

...}
AND N;Cl

.9

I5-3

Fruor

‘ ...“.-

I
o‘
I.
I

 

CORROSIVE 5;. F‘ECTS OF H10, CLCIZ'I‘VIZCIZ

' AND mca AT 35°F LNOT AERATED)

FIGURE I5-4
-57- _

 

:L
S:
u
, 'F
5'
. 57)..
. .;_'_ ,
‘ ...“. “1%
' ~’-‘-.U'.av-
_ .
V

t ERIES I3

CORROSIVE EFFECTS OF H20, C&CI2-M3CIZ
' ANO N.CI AT 35°F (NOT AERATED)
FIGURE I5-5

.‘."FFF'F(F&£:F[Fv/'r I)"
1‘ ‘_ I FV.F\ ,k'FF\ho.

AND NaCl

'— 7“?”"Fvv‘
IL?" I

 

“Pram

‘. \J

OF H,O,CaCI2.“I“733‘2
AT 35°F (AERATED)
FIGURE:- '5'2

 

 

4

N... v

AND N;CI AT 35°F (AERATED)

FIGURE l6‘3

-6'-

 

,. ...—WW .—

I

, CaICI

O

)
D
E
_.I

z A

H R
E

F A

AV (\

9 ..r

T u.

C

E 3

F

F m

E

E C

I a

H... N

A D

N.

Am A

mp.

C

C

FI’Z'IRE I6'4

‘. I
I; .

’ \ 1'-

I . '.
‘0!..b.t.. -. - -a..-. ov

 

l
g S"’RIES I4 .
I; ‘ ..

CORROSIVE EFFECTS OF H,O,CaCIz—MSCIZ
AND N.CI AT 35°F (AERATED)

C'Iffit IDF‘ [6—5
-63..

 

 

'2

CaC

AND NaCI AT 75°F (AERATED)

H20)

FFECTS OF

CORROSIVE E

FIGURE I7-I

-64—

 

I

. ..~...H.I N1
«J.
y

\

I
v
r
.

9

I. I
O.\
I\

I.“

\W

 

IJOII

ii

.HI.

.6

CORROSIVE EFFECTS OF HzO,C

AND NaCl AT 75°F (AERATED)

FIGURE I7-2

-65.-

 

 

.I
. v? .13.
75%... AI] \ .

\Wum..\‘l...u.u mK‘ .
. \I I I \ \‘IVW‘V
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a ,s

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.I..\

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t I." r. nu‘nl

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.. v (\t \v.
.I ......

.0
J

a .

 

ISCIz

"IN

OF H20, CQCIZ

AND NaCl AT 75°F (AERATED)

FFEC"

E

CORROSIVE

”‘3
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'-
n

 

 

an“ 1

l .

I

Yank?"

.

43m
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4.‘

‘r «usual 50‘-

 

 

3

I5

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.._)

,. ....r at . ......I

, CaC

zO

" T5 OF H
AND NaCl AT 75°F (AERATED)

/‘
K
V

O"
y.

F

E

O

HGUREI7-4

 

3.. x
.74.

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CORROSIVE

 

 

 

 

9-A IO'-A

 

SERIES I5

_ v —r--v—.o .- -an- .-M

ru-"1\"—"‘~'wm.' .r. -. ~ .‘ ~ T;-‘r“\.-- ~ «' w“ “umM-‘rq""v"*“"-

CORROSIVE EFFECTS OF H,O,C.CIz—M3CI,_

AND NaCl AT 75°F (AERATED)
FIGURE I7-5
—68-

 

I SERIES l6

CORROSIVE EFFECTS OF HZO,CaCIZ-MSCI2
AND NaCI AT 75°F (NOT AERATED)
FEG'JRE I8-I

..69‘.

 

 

--—-, >v

CORROSIVE EFFECTS OF HZO,CaCI-‘._~?/3(;IZ
AND NaCl AT 75°F (NOT AERATED)
FIGURE [8-2

 

r-—-v—-

SERIES I8

,-._, ___...... M
x

CORROSIVE EFFECTS OF HZO,CaCIz-MSCIZ
AND NaCl AT 75°F (NOT AERATED)
FICLJRE I8-3
-7'-

 

l SERIES I6

 

CORROSIVE EFFECTS OF HzO,CaCIz-—M3CI1

AND NaCl AT 75°F (NOT AERATED)
FIGURE Ia-4
-72—

C . .
. .4- An>o~— ng-~..-. o~ -..-...“.

IO-A

 

 

 

a--- ._ -7

CORROSIVE EFFECTS OF HzO,CaClz-M3CI,_
AND NaCl AT 75°F (NOT AERATED)

HGUREIB-S
-73-

APPENDIX B

LABORATORX PROCEDURE

1 II
The solutions were prepared by weighing out the amount of chlor-
ide salt necessary to obtain the desired concentration and adding
enough distilled water to bring the volume up to 500 m1. In the
event that the chloride salt was in.brine form, the brine was
measured volumetrically and diluted to the desired concentration with
distilled water. The salts used were, in all cases, the technical
grades used in highway applications. Inhibitors, when used, were
'weighed out and placed in this solution. All inhibitor concentrations
'were based on the total chloride salt content of the solution.
e at o Plat

The metal used was 19 gauge, S.A.E. No. 1008 sheet steel, which

I-

 

Figure 19. Freshly prepared test plates.

-75-

was the same as that used in the 1947—1949 Oldsmobile bodies. The

metal was cut into plates 2 in. by 2 in. A l/4 in. diameter hole was

drilled through the plates near one edge in such a manner as to leave

no burrs around the hole. The plates were then polished with No. 280

wet and dry emery paper and finally with crocus cloth to produce a

uniform surface, (see Note). The plates were then cleaned in carbon

tetrachloride or trichlorethylene to remove any grease or oil from

handling, dried in an oven at 220° F. for one hour and weighed to

constant weight .

Note: Sand-blasting may be substituted for the above polishing method,

providing it is used throughout the experiment.

Tests
The tests were run according to one of the following cycles.

Since pH control on the highway did not seem feasible, no attempt at

pH control was made in the laboratory. However, the pH was checked

periodically throughout the tests. The inhibitor was not replenished

during the test, since it was desired to learn how long a given

application of inhibitor would remain effective. Triplicate samples

[were run in all cases. The amount of corrosion was calculated in

milligrams per square decimater and in milligrams per square decimeter

per day, using the equations given on pp. 80.

WM

500 m1. of prepared solution were placed in a 400 ml. beaker and
the weighed metal plate suSpended in the solution by means of a glass

hook. The solutions were kept saturated with oxygen by continuously
bubbling filtered airthrough the solution, which also supplied agita-
tion. The beaker was kept covered insofar as possible, to reduce

~76-

evaporation losses and to keep dust and other foreign material from
entering. Any evaporation losses were made up by adding distilled

water periodically in order to maintain the solution volume at 500 m1.

Tests were run at 75 1 5° F. and at 55 : 2° F.

The metal plate was removed from the solution at 7 day intervals,

cleaned, dried at 220° F. for one hour, weighed to constant weight and
returned to the solution. The cleaning was done by thoroughly brushing
with a stiff bristle or brass brush under a stream of water in order to

remove as much of the corrosion products as possible. The duration of

 

Figure 20. Detailed Set-up for Corrosion Cycle No. 1.

-77.

 

Figure 21. Battery of Tests for Corrosion Cycle No. l.
'the test was 28 days.

Corrosion Cycle No. 2

500 ml. of prepared solution were placed in a 400 ml. beaker and
the weighed metal plate placed in the beaker with one edge resting on

the bottom of the beaker and the top of the plate leaning against

the side of the beaker. The beaker was covered with a glass plate to

exclude foreign matter, but in such a way as to allow air circulation

over the beaker. The plate was alternately immersed and exposed to

air as follows:

16 hours - immersion
2 hours air exposure
4 hours - immersion
2 hours - air exposure

The plate was removed from the solution at 7 day intervals, cleaned,

weighed, and returned to the solution as in Cycle No. l. The duration

-73-

 

of the test was 28 days. Temperature was 75 : 5° F.

Corrogign ngle Hg, 5

The solution was prepared as previously stated, except that the
distilled water was freshly boiled for 15 minutes to remove dissolved

oxygen before preparing the solution. The prepared solution and

weighed metal plate were placed, as described in Cycle No. 2, in a

16 ounce specimen bottle and the cap tightened to limit the oxygen

supply. The plate was cleaned and weighed at the end of the test

only, using the cleaning method of Cycles No. l and 2.

Tests were
runat 7515° F. andat 55:2‘1“.

 

Figure 220

Detailed Set-up for Corrosion Cycle No. 5.

-79-

ECUATIONS USED FOR CORROSION CALCULATIONS

General Eggtions

Corrosion Rate = 1000 W" in mg/dmZ/day
A t

Cumulative Corrosion = 1000 W in mg/dm2
A

W

Corrosion Rate = 1000 W = 1854 W

0.54 t t

Cumulative Corrosion = 1000 W = 1854 W
0.54

For Series 15 to 16, Inclusive

I .

Corrosion Rate = 1000 W = 2085 _E;
0.48 t, t
Cumulative Corrosion = 1000 W’ = 2085 W
0.48
A == Average total surface area of test plate. (dmz)
W == Weight'loss which occurred during time interval "t". (gms)
t == Time during which corrosion took place. (days)

~80—

TABLE 13

ANALYSES OF CALCIUM CHLORIDE BRINES USED FOR CORROSION STUDIES

 

No. 1 No. 2 No. 5

 

Calcium Chloride, per cent by weight 57.48 40.57 59.78
Magnesium Chloride, per cent by weight 1.54 1.76 1.47
Sodium Chloride, per cent by weight 0.99 0.51 0.56

Specific Gravity 25.0/25.0° c. 1.599 1.451 1.422

Sum of Calcium and Magnesium Chlorides 59.02 42.55 41.25

 

These brines were obtained from Michigan Chemical Co., St. Louis,
Michigan. Analyzed by the Solvay Method.

The Rock Salt used in these tests was obtained from the Michigan
State Highway Department, and was identical to that used on highways.

-81-

TABLE 14

CHLORIDE CONTENT OF WINTER ROAD SLUSH

 

 

Sample Location ' Sample Temp. CaCl
No. (° F.) (Wt. %)
1 Cr. River-Abbott Rd-center of intersection 52.0 0.28
2 " " " " right gutter, east bound 51.5 0.50
5 " " " " left gutter, east bound 52.2 0.59
4 " " " " right gutter, west bound 51.5 1.52
5 Mich. Ave.-De1ta St-right gutter, west bound 51.8 0.41
6 “ " " " -center of intersection 51.6 0.24
7 5 " Beal St.-right gutter, west bound 50.8 1.47
8 " " " " left gutter, west bound 51.9 0.50
9 " " " ” center of intersection 50.7 1.24

 

These samples were taken about 6 hours after application of a calcium
chloride-sand mixture to the streets of East Lansing, Michigan. Air
Temperature = 28° F., February 16, 1949. Pavements. Concrete.

-32-

TABLE 16
MEASUREMENTS TO DETERMINE AVERAGE TOTAL PLATE AREA FOR CORROSION TEST

SERIES NO. 15—16, INCLUSIVE

Dimensions of Sampled Plates

 

 

Length . Width Thickness Hole Diameter
(in.) (in.) (in.) I (in.)
1.86 1.86 0.044 0.250
1.91 1.91 0.044 0.250
1.91 .1.90 0.044 0.250
1.91 1.90 0.044 0.250
1.86 1.86 0.044 0.250
1.91 1.91 0.044 0.250
1.91 1.91 0.044 0.250
1.91 1.90 0.044 0.250
1.88 1.84 0.044 0.250
1.90 1.91 0.044 0.250

Mean 1.90 1.89 0.044 0.250
Face.Area = 2(1.90)(1.89) - (0.g§)2 = 7.08 in.2
4
Edge Area = 2(1.90 + 1.89)(0.044) + (0.25)(0.044) = 0.55 in.2
.Average Total Area = 7.08 + 0.55 = 7.41 in.2
2 - 2 2
1 in. - 0.0645 dm Average Total Area = 0.48 dm

~84-

 

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TABLB :F7
pH (BECKHAN)

Speoiun - 8.r1e. 13 Series 14 Series 15 Series 16
No. Etta-1114 days Initiallllt day. Initial! 14 days Initial 14 days
13 6.60 7.58 6.62 7.28 7.00 7.05 7.00 7.70
1b 7.00 7.43 7.00 7.30 6.79 7.10 6.80 7.58
10 6.70 7.35 6.80 7.30 6.62 7.58 6.72 7.52
2‘ 8.40 7.31 8.40 6.25 8.40 6.90 8.40 8.22
2b 8.40 7.20 8.40 6.79 8.40 6.99 8.40 8.41
20 8.40 8.04 8.40 6.82 8.40 6.93 8.40 7.00
3C 8.10 8.40 8.10 7.70 8.10 6.20 8.10 7.46
3b 8.10 8.33 8.10 7.72 8.10 5.97 8.10 8.68
30 8.10 8.15 8.10 7.02 8.10 5.87 8.10 8.59
4C 7.90 7.70 7.90 6.80 7.90 6.44 7.90 8.09
4b 7.90 7.95 7.90 v6.48‘ 7.90 6.40 7.90 8.08
40 7.90 7.90 7.90 7.72 7.90 6.42 7.90 8.09
St 7.70 7.60 7.70 6.69 7.70 6.18 7.70 7.59
5b 7.70 7.69 7.70 6.68 7.70 6.14 7.70 8.01
50 7.70 7.66 7.70 6.64 7.70 6.14 7.70 7.80
6. 7.30 8.12 7.10 7.45 7.35 7.18 7.20 8.15
6b 7.30 7.48 7.30 7.50 7.10 7.04 7.10 8.20
60 7.30 7.30 7.20 7.64 7.15 7.03 7.00 7.99
7‘ 7.25 7.19 7.30 7.19. 7.30 7.03 7.30 9.00
7b 7.25 6.98 7.30 7.32 7.30 7.00 7.30 9.30
70 7.25 7.00 7.30 7.32 7.30 7.00 7.30 9.10
8. 7.45 6.63 7.25 7.49 7.25 6.72 7.25 8.42
8b 7.45 6.65 7.25 7.30 7.25 6.43 7.25 9.19
80 7.45 6.50 7.25 7.12 7.25 6.66 7.25 9.32
9. 7.60 6.35 7.45 7.02 7.45 6.04 7.45 9.50
9b 7.60 6.25 7.45 6.90 7.45 6.10 7.45 9.20
90 7.60 6.98 7.45 6.84 7.45 6.35 7.45 9.32

10. 7.60 7.42 7.60 7.11 7.60 6.98
10b 7.60 7.58 7.60 7.00. 7.60 7.58
100 7.60 7.50 7.60 6.97 7.60 7.98

~109-

 

5.

4.

5.

9.

10.

ll.

15.

14.

15.

SELECTED REFERENCES

Warner, C. D., "Does Salt Damage Autos", American City, 92-5,
August, 1947.

”Chromates Lessen Corrosion, Goodyear Says",

Michigan Roads and Construction, 14, January 1, 1948.

"Akron Experiments with Rust Inhibitor", Engineer-
ing Megs Record, 99, 59, January 22, 1948.

Brown, J. H. and Friend, J. 1., "The Action of Salt Solutions and
of Sea water on Iron at Various Temperatures”, Jogrg.
Chem. Soc., (London) 99, 1502,1911.

Haering, D. W., "Refrigerating Brines", Power Plant Engineer, 44,
71-2, 1940.

Evans, U. R., "Corrosion and Refrigeration", Ice and Cold Storage,
.§9, 180,1956.

Speller, F. N., Corrosion Gauges and Prevention, McGraw—Hill Book
00., 2nd. Ed., 1955, 149. '

walker, W. H., "The Function of Oxygen in the Corrosion of Metals",
Trans, Electrochem, Soc., 14, 175—187, 1908.

Uhlig, H. H., Co sion Handbook, John Wiley and Sons, Inc., 1st
Ed.’ 1948, 9.

Darrin, Marc, "Chromate Corrosion Inhibitors in Bimetallic
systems", Ind, and Eng. Chem” (Anal. Ed.) 1;, 755-59, 1941.

Evans, U. R., Metallic Corrosion, Passivitz and Protection, Edward
Arnold 00., 1948, 269-271.

Evans and Hoar, "The Passivity of Metals, Pt. VII, The Specific
Functions of Chromates", Journ. Chem, Soc., (London)
2476-81, 1952.

Finney, E. 1., “A Microscopic Examination of Scaled and Unsealed
Concrete", Mich, Eng. Exn. St§,_Bu11, No, 101, Michigan
State College, 1944.

Hatch, G. B. and Rice, 0., "Corrosion Control with Threshold
Treatment", Ind , and Eng, Cheg.,.§z, 741-49, 1945.

Darrin, Hare, ”Chromate Corrosion Inhibitors in Bimetallic Systems",

-110—

16. Sangster, S. E., I‘See End to Car Nemesis-Sa1t", Motor News; April,
1 ‘ 1949.

17. Davis, Russell and Whitman, ”The Solubility of Ferrous Hydroxide
and Its Effect Upon Corrosion", Journ. Am, Chem. Sog.,.gz,
70-79, 1925.

18. Speller, F. N., 93. g;§., 248.

19. Ibid., 250.

20. Ibid., 251.

21. Ibgd., 165.

22. Ibid., 155.

—111-

SUPPLEMENTARY BIBLIOGRAPHY

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Dill, C. and walker, W. B., "The Effect of Stress Upon the Electro-
motive Force of Soft Iron”, Trans. Am. Electrochem. Soc.,‘;;,
155, 1907.

Smith, M. B., "Air as a Stimulator of Corrosion in Refrigerating Brines",
Eng, News, _6_§_ 1002—5, 1915.

Atchison, L., "The Theory of the Corrosion of Steel", Jo Iron and
Steel Ins§., (advance c0py) 1916.

Cushman, A. S., "Electrolytic Theory of the Corrosion of Iron", Trans.
Am, Electrochem, Soc., 12, 405-408.

Thompson, T. 0., ”Preservation of Iron and Steel by Means of Passivi—
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Richardson, E. A. and Richardson, L. T., “Corrosion of Cast Iron and
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Fleming, W. R., "Corrosion of Iron in Water, Pure Water and Air Com-
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Rudnick, P., "Corrosion Tests on Commercial Calcium Chloride Used in

Automobile Anti-freeze Solutions", Journ, Ind, and Eng, Chem.,
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Speller, F. N., "Abatement of Corrosion in Central Heating Systems",
Bur, Mines Tech, Paper 256, 1919.

Isaacs, A. and McKelvy, E. 0., “Causes and Prevention of the Formation

of‘Non-Condensible Gases in Ammonia-Absorption Refrigerating
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McDermet, J. R., "Interpretation of Boiler4Water Analyses", Chem, Age,
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Speller, F. N., “Control of Corrosion in Refrigeration Systems", Jogrg.
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"Anti—Corrosive Preparations for Iron and Steel", Ch .
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-112-

Evans, U. R., "Passivity and Overpotential",[Eggns,_Faragay Soc.,
(advance proof), February 15, 1922.

Friend, J. N., aThe Influence of Strain Upon the Incorrodibility of

Iron and Steel", 5rd (Interim) Rgport of Comm. of the Inst.
of Cizil Eng., (London) 1925.

Hall, W. T., "The Mechanism of the Corrosion of Iron", Ind. Eng. Chem.,
l5. 426-27, 1925.

Johnston, J., uThe Mechanism of Corrosion", Ind. En Chem.,.lé, 904-5,
1925.

Wilson, R. E., "The Mechanism of the Corrosion of Iron", Ind, Eng.
Chem., l5, 427, 1925.

Bancroft, W. D., "The Electrolytic Theory of Corrosion", Journ P 3
Chem., ..2.§., 785‘871, 1924.

Evans, U. B., ”The Mechanism of Busting of Iron", Proc, Cambridgg Phil.
Soc., 22, 54-55, 1924.

Bentley, J. L., Friend, J. N. and Wost, N., "The Mechanism of Corro-

Clare, McHaffie, and Shipley, "Corrosion of Iron in the Absence of
Oxygen", Ind, and Eng, Chem.,.lz, 580-81, 1925.

Hadfield, R. and Morrell, R. 8., ”Protective Paint Coatings", Journ.
0;; 00193; Chem,.Assgg.,.§, 5-25, 1925.

Hatfield, W. H., "Modern Developments in Steel Resistant to Corrosion”,

Speller, F. N., "A Study of the Corrosion Factors and Electrochemical
Theory", d d En C .,‘l1, 559-46, 1925.

Evans, U. R,, ”The Fundamental Principles of Corrosion", Me Ind.,
(London) 23, 150-52, 1926.

Gunderson, L. 0., "Corrosion, An Electrochemical Phenomenon?, 31, Rev.,
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Pierre, L., "Corrosion (of Pipes) by Salt Brines", Brasserie et Malterie,
l6. 155—40, 1926.

Scheiber, J. H., ”The Chemical Reaction of the Busting of Iron", Farbe

Whitman, w. G., "Corrosion of Iron", Chem. Rev., g, 421—55, 1926.

~115-

Zelger, C., "Protection of Iron Against Corrosion by Calcium Chloride
Brine", Chimie et Industrie, Spec. No. 249, September, 1926.

Bengough, G. D., Lee, A. R., and Stuart, J. N.,"Theory of Metallic
Corrosion in the Light of Quantitative Measurements", Proc.
qu. Soc., (London) 116A, 425-67, 1927.

Chappell, E. L.4 Roberts,fJ. K..and Russell, R. P., ”Corrosion in the
Refrigeration Industry", Refrig, Eng.,.l§, 209-19, 1927.

Stumpe, R., "Contribution to the Theory of the Processes of Corrosion",
Korrosign u. Metallschutz,.§, 169-71, 1927.

Gibbs, R. E., "Decreasing Corrosion in the Ice Tank", Power, §1, 1020-
1025, 1928.

Lincoln, H. L., l'Corrosion in Ice Plants", Power,.§1, 688-89, 1928.

Brownlie, 13., "The Pickling and Cleaning of Metals, II and III; Some
Considerations of the Chemical Reactions Involved", Sheet
Metal Igd., g, 425-27, 1950.

Liebreich, E., and Haas, E., "Supplementary Studies of the Evans
Theory", Egrgosigg g, Metallschutz,.§, 549-55, 1950.

Masing, C., "Fundamentals of Corrosion", Z, Mgtallgggde,‘gg, 521-26,
1950. '

Medinger, R., ”Brine for Refrigerators, etc.", (Austrian) 12;, 988,
November 15, 1950.

Wheaton, R. S., 'Corrosion Prevention Methods in Brine Tanks and Ice-
Making Tanks", Power, 15, 857-58, 1952.

 

Hudson, J. C., "Experimental Methods for the Study of Corrosion" ,
Journ, Soc. Chem, Ind.,._g, 69-76,1955.

Colbeck, E. N., Crovent, S. N., and Fleming, F. L., ”Experiments with
Treatment of Calcium Chloride Brine with Sodium Chromate for

Prevention of Corrosion", Ice and Cold Stogage,.§g, 180-81,
1956.

Evans, U. R., ”Corrosion and Refrigeration", Ice and Cold Storage,
fi,180, 1956 0‘

L
Idoux, L., "Protection Against Corrosion of Iron by Brines",lBgll.
Assoc, Chim., 5, 261-66, 1956.

Haering, D. N., "Film Inhibitors in Industrial Aqueous Systems",
Ind. Eng, Chem,,ԤQ, 1556-61, 1958.

Machu, N., "Inhibiting of Acid Corrosion by Means of Organic Substances"
Angew. Chem.,‘él, 855-57, 1958.

~114-

Pourbaux, M., "Thermodynamics and Corrosion", Metaux et Corrosion, 15,
189-95, 1958. .

Watts, 0. P., "Corrosion of Metals", U. of Wisconsin Exp, Sta. Bu11.,
Ser. No. 85, 1958. ‘

Muller, W. J., ”Passivity and Corrosion of Metals”, Kglloid—Z.,‘§§,
150-66, 1959.

Haering, D. N., "Refrigerating Brines", Power_Plant Eng.,.gg, 71-2, 1940.

Newzig, H. and Reschke, L., ”Investigation of the Inhibiting Action of
Potassium Permanganate and Sodium Chromate in the Attack of
Aluminum by Sodium Hydroxide“, Aluminum, 25, 558-62, 1940.

Tseitlin, Kh. L., ”Influence of Reducible Organic Compounds on Corro-
sion of Metals by Inorganic Agents”, Org, Chem, Ind., (U.S.S.R.),
1, 105-105, 1940.

Darrin, Marc, uChromate Corrosion Inhibitors", Proc, Ann. water Conf.

Koritnig, 0. T.y "Protection of Brine Systems Against Corrosion",
Milchw, Zentr.,'ZQ, 9-10, 1941.

Evans, U. R., "Distribution of.Attack on Iron or Zinc Partly Immersed
in Chloride Solutions", Nature, 150, 1942.

Kalpers, B., ”Corrosion Protection of Steel by Chromium Diffusion",
Korrosion u. Metallschustz,.1§, 256-58, 1942.

Fink, C., Paul, C., and Turner, W., "Zinc Fellow in the Inhibition of
Corrosion-Fatigue of Steel in NaCl Solution", Trans. Electro-

ghem, Soc., 85, 25(preprint) 1945.

Machu, W., "Layer Theory of Passivity, Theory of Inhibitors and Phos-
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Warner, J. C., ”Thermodynamic Considerations in the Corrosion of Metals",
Traps, Electrochem, Soc.,.gfi, (preprint), 1945.

Pope, G. A., 'An Adjusted.Brine Checks Corrosion", Power, 88, 569, June,
1944.

Akimov, G. V., Glukhova, A. I., "The Rate of Corrosion of Aluminum and
on the pH of the Solution", Cgmpt, Rend. Aca, Sci., (U.S.S.R.),
39, 194-97, 1945.

LaQue, F. L., and Knapp, B. B., "Planning and Interpreting Corrosion
Tests", Corrosiog and Material Protection, 25 17-25, 1945.

-115-

Thornhill, R. S., "Zinc, Manganese, and Chromium Salts as Corrosion

Inhibitors", Ind. and Eng. Chem.,.fiz 706-9, 1945.

Darrin, Marc, ”Chromate Corrosion Inhibitors in Chloride Systems";

"Rate of Consumption of Chromate", Ind. and Eng, Chem.,
.58, 568-75, 1946.

Shepard, S. W., "Corrosion Testing in a Chemical Plant", Chem. and Met.,

NO;
1,750,761

2,187,725

2,207,767

2,215,058

2,274,058

2,297,551

2,519,667

2,554,774

2,575,958

2,426,496

Egg.,.5§, 217-26, 1946.

IEHIBITOR PATENTS

- Otto 7. Martin (to the Martin-Calvin Co.) Excess Mg(OH)2

maintained in brines in contact with iron.

F. N. Alquist and H. R. Slagh (to Dow Chem. 00;) Certain
types of organic amines for prevention of corrosion of
iron by HCl solutions.

W. 0. Turner. Corrosiveness of drip brines reduced by
addition of a chromate.

T. S. Hodgins and A. G. Hovey (to Reichold Chem. 00.).
Manufacture and use of certain aminohydroxy compounds
for rust prevention.

M. T. Goebel and I. F. Walker (to DuPont Co.) Production
of long-chain metallonitriles suitable for use in
corrosion prevention.

L. H. Bock (to Rohm and Haas Co.) Preparation of tertiary
amines suitable for corrosion inhibitors.

-‘Au M. Edmunds (to Dow Chemical 00.) Sodium Arsenite used

for inhibitor in Ca012 solutions.

- A. R. Rummelsburg (to Hercules Powder Co.) Esters used

as rust inhibitors.

-.A. W. Burwell (to Alox Corp.) Nitriles, amino acids and

their condensation products used as corrosion inhibitors
in oils.

F. F. Farley (to Shell Development Co.) Alkali metal salts

of long-chain dibasic acids used as corrosion inhibitors in
antifreezes, deicing fluids and metal treating compounds.

-116-