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British Corrosion Journal

ISSN: 0007-0599 (Print) (Online) Journal homepage: http://www.tandfonline.com/loi/ycst19

Criteria of Soil Aggressiveness Towards Buried


Metals. I. Experimental Methods

G. H. Booth, A. W. Cooper, Pamela M. Cooper & D. S. Wakerley

To cite this article: G. H. Booth, A. W. Cooper, Pamela M. Cooper & D. S. Wakerley (1967)
Criteria of Soil Aggressiveness Towards Buried Metals. I. Experimental Methods, British
Corrosion Journal, 2:3, 104-108, DOI: 10.1179/000705967798326957

To link to this article: http://dx.doi.org/10.1179/000705967798326957

Published online: 18 Jul 2013.

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CRITERIA OF SOIL AGGRESSIVENESS TOWARDS
BURIED METALS. I. EXPERIMENTAL METHODS
By G. H. BOOTH,* A. W. COOPER,* PAMELA M. COOPER* and D. S. WAKERLEY*

Experimental.d~tailsand .specime!1results ~re givenfor a number of field and laboratory tests for some of
the ch~ractenstlc pro~ertles of s.ollsthat mIght be expected to have some relation to the aggressivenessof
the sOlIstow.ards buned (espectal~y,ferrous) metals. Properties examined include electrical resistivity,
redox~potenttal,.water and soluble Iron contents, pH and various factors bearing on the activity of sulphate
reducmg bactena.

Introduction analysis. Tomashov & Mikhailovsky7 have emphasised the


The corrosion of metallic structures buried in, or in contact inlportance of water content and Stratfull8 has shown an
with~ soils has been a serious engineering and economic optimum water content to give a minimum resistivity that
problem for many years. As long ago as 1949, the results of can be correlated with aggressiveness. Romanoff4 considers
past omissions in the provision of adequate protection to that the conclusions of other workers on the relation of 'long-
pipes laid in aggressive soils were stressed by Butlin & line' currents set up in pipelines by concentration-cell and
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Vernon.l In 1948, an estimate was made of the cost, from differential-aeration effects are contradictory and that, in
actual destruction and of preventative measures, to the U.S. general, corrosion from this source is not serious. Tomashov
pipeline industry2 and this amounted to $600 million annually, & Mikhailovsky9 have challenged this view and emphasise the
while in 1956, Vernon3 estimated that in the U.K. the cost of importance of this effect. Starkey & Wight10 have shown
underground pipeline maintenance and repair was about that acidic soils are unfavourable for anaerobic (microbial)
£20 million annually. In the absence of even approximate corrosion and claim that the redox-potential is the most
information on the possible aggressiveness of the soil environ- significant factor indicative of probable aggressiveness from
ment, when, for example, a pipeline is being laid, the engineer this cause. Laboratory work on corrosion of steel by pure
is faced with two alternatives. He can either prepare for the cultures of sulphate-reducing bacteria has led us to believell
worst by installing a comprehensive protection system from that the concentration of soluble iron in a soil may sig-
the outset and correspondingly increase the cost of installation, nificantly affect the severity of bacterial attack.
or he may take the risk of having to re-excavate and repair or Many workers have suggested field and laboratory tests
replace at some time in the future. The latter course will not for the assessment of single contributory factors towards
only entail very high labol;lr costs, but may also involve loss of soil aggressiveness but, as Tomashov & Mikhailovsky9 have
production while the installation is out of commission for pointed out, there exists no single comprehensive test that
maintenance. It is therefore of considerable economic im- will completely characterise a soil. However, an attempt has
portance that the potential aggressiveness of a soil should be been made to devise a scheme of testing, keeping the number
known before metallic structures are buried. of tests to a minimum and the execution and instrumentation
Factors that might be expected to influence the corrosion as simple as possible, that will indicate probable aggressive-
of metals in soils are many and involve properties both of the ness of an unknown soil to an extent that is useful and
metals themselves and of the soil environment. This work practicable to the engineer. In this paper, testing methods
is concerned 'solely with the environmental factors. Butlin & are described. In later publications, the results of the tests
Vernonl list six principal causes of external corrosion of when applied to soils, the corrosion history of which is to some
buried metal pipes (some mutually exclusive but others that extent known, will be assessed and the prognoses of aggressive-
may operate simultaneously). Of these, four may be con- ness of a number of selected soils will be compared with the
sidered to be characteristics of the soil, namely anaerobic results of burial tests. Throughout, the emphasis is on the
bacteria, the chemical nature of the soil particularly acidity behaviour of iron and steel but some information on the
and the salt content, differential aeration, and concentration behaviour of some common non-ferrous metals has been
cells. Romanoff4 classifies corrosive factors under the four included.
headings of aeration, electrolyte, electrical factors, and
miscellaneous, the last group containing man-made alterations Selection and Experimental Details of Test Methods
to the natural soil environment and the effect of bacteria. The tests employed fell into two main groups, those
Many workers have demonstrated a correlation between the conducted in situ and those using samples returned from the
corrosion occurring in soils and individual or small groups of field to the laboratory.
the possible influencing factors. For example, Romanoff4
has stated that measurements of electrical resistivity give
better correlation than pH or total acidity. Denison & Field Tests
Ewing5 have shown a relationship between corrosion and From a consideration of previous work, two tests were
resistivity and/or total acidity. Smith6 has shown that many selected for direct application in the field, one (soil resistivity)
inconsistencies appear when corrosion is related to chemical as a possible measure of the likelihood of oxidative corrosion
the other (redox-potential) being considered indicative of th~
* Metallurgy Division, National Physical Laboratory, Tedding- risk of bacterial corrosion. The measurement of redox-
ton, Middlesex. . potential requires also a measurement of pH and it was
Manuscript received 27 January, 1967 found by experience that the direct measurement of pH in the

Br. Corros. J., 1967, Vol. 2, May


Booth et al.: Criteria of Soil Aggressiveness towards Buried Metals. I. 105
field was unreliable except in extremely wet soils. pH was 15

therefore determined in the laboratory. All field tests were


carried out as close as possible to installations of known
history.
Resistivity The Wenner four-terminal method12 and a 10
Nash & Thompson 'Tellohm' soil resistance meter (Corrosion
model) were used to measure the average bulk resistivity of
the soil over a range of depths from 2-!- to 15 ft. The average £
f-
0-
value for a depth of 3 ft was interpolated from a plot of W
C

resistivity against depth (Fig. 1). The method was very


reliable and gave reproducible values throughout the range
6-40,OOOQ-cm.
Redox-potential Initially, a probe similar to that described
by Deuber & Deuber13 was used, but this was soon found to
be too fragile for use in any but the softest soils. A more 1000 1500 2000 2500
robust model was designed (Fig. 2). The most important RESISTIVITY, n -em
modification was the removal of the reference electrode from Fig. 1. Variation of soil resistivity with depth
the hollow stem of the probe to enable a solid stem to be
Site: Fortis Green; soil: light-brown clay, some 'make-up';
used. A separate saturated calomel reference electrode was history: aggressive to ferrous metals
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Nose piece
joined to rod with
araldite

+ 0'05
40
0

Pt electrod~

.S
co
.M
"8 in groove

22 s.wg. Cu wire Cu wire


encased in araldite

pt/Cu wire
junction

22 s.w.g. ~1in
Pt wire !ifein Pt wire

3~2in
.S; Platinum ~
eloc!rade • .-.

Cross-section of nose pi(ZCe

Fig. 2. Redox probe

Br. Corros. J., 1967, Vol. 2, May


106 Booth et al.: Criteria of Soil Aggressiveness towards Buried M eta/so I.
used in conjunction with a portable transistorised pH/milli- made from this, all in triplicate. The cultures were in-
voltmeter. For all measurements, the reference electrode was cubated at 30° in McIntosh & Fildes anaerobic jars in an
inserted in the soil at a distance of 1 ft from the probe. atmosphere of 99 %H2/1 %C02 for two weeks. The total
Differences in potential of up to 10 mV could be recorded viable count was calculated from the highest dilution at
when this distance was varied from 1 inch to 3 ft but the which all three of the triplicates showed blackening. The
variation with distance was irregular. The readings from the incubation period of two weeks was found by experience to
duplicate platinum electrodes of the probe generally agreed be the optimum.
to within about 0·01 V. Differences greater than this Hydrogen uptake. Since cathodic depolarisation by micro-
indicated that the platinum required cleaning. Gentle organisms plays an essential role in the bacterial corrosion of
abrasion with a scouring powder, and washing in 70% iron and steel,17,18it was thought that a direct measurement
alcohol and then with distilled water were found to give of the ability of a soil to take up hydrogen might give a simple
reliable results. Drifting and/or erratic readings were indication of bacterial aggressiveness. A simple differential
avoided by rotating the probe through 360° in the soil at the manometric apparatus, shown diagrammatically in Fig. 3,
same time pressing firmly on the handle. The redox- was used. 30 g (wet weight) of soil was incubated at 25° for
potential was calculated from the observations by the 14 days in an atmosphere of hydrogen, and the volume of H2
relationship13 absorbed was measured.
En = E +0'250 +0'060 [pH - 7] pH. A standard procedure was adopted. 20 g soil (wet
where En = redox potential at pH = 7 (V, standard hydrogen weight) were slurried with 50 ml distilled water and the pH
scale). was· determined electrometrically using a glass electrode and
E = mean of the potential observed from the two platinum saturated calomel reference electrode. The soil was not
dried initially since Romanoff19 has shown that such treat-
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electrodes (V).
me~t may reduce the pH value of the subsequent slurry by
up to 3· 5 units. The above concentration of slurry was
Laboratory tests chosen for convenience since it gave a manageable system for
Laboratory tests were conducted on a total bulk sample of all the soil types tested. The effect of varying the concentra-
about 500 g of soil taken from a depth of 3 ft and put into tion of the slurry was investigated for one particular soil only;
clean polystyrene jars with tightly fitting lids. No special
precautions were taken to exclude air, but the jars were filled
as completely as possible and stored at 4°. Six tests were
then performed on each sample, one specifically relative to
oxidative corrosion, three to bacterial corrosion and two
probably relative to both.
Water content. Approximately 5 g of soil were weighed
and dried to constant weight in an air oven at 100°. The
results were expressed as percentage water, based on the
wet weight of the sample.
'Bottle test'. This test has been used without very great
confidence for many years at the former National Chemical
Sr>il
Laboratory as a test for potential bacterial aggressiveness of sample
Thermobar
soils. A development of the test has been proposed by Hoar
& Farrer14 in an attempt to define an 'activity index', but the
method has been criticised.l5 The original test was included
in this survey particularly to ascertain its limitations.
Approximately 2 g of soil were incubated at 30° in a 10 ml
screw-capped bottle completely filled with Baars' medium16 Water
seal
supplemented with 0·05 % ferrous ammonium sulphate as
indicator, and the number of days for blackening to occur
was recorded. In one series of tests, no additional aids to
growth such as the. inclusion of yeast extract or a redox- Gas Brine
burette reservoir
potential poising-agent in the medium were employed. In a
parallel series of tests, O·1% L-cysteine hydrochloride was
included in the medium to poise the redox-potential at about
-0·14 V. The pH of all media was adjusted to 7'2-7·4
before they were added to the soil; no subsequent pH adjust-
Brine
ment was made.
Total viable count of sulphate-reducing bacteria. This test --
was included on the precept that bacterial corrosion might be
related to the total number of viable sulphate-reducing
organisms initially present in the soil. The count was ob- --
tained from serial dilutions of soil in Baars' medium supple- ~ -------= = ~-----------------
mented with O·1% yeast extract, O·05 % ferrous ammonium
sulphate and 0·1 % sodium dithionate (to poise the redox-
potential at -0·4 V), the final pH of the medium being
7'2-7-4. An initial dilution was made of 10 g (wet weight)
of soil in 90 ml medium and ten seriall-in-10 dilutions were Fig. 3. Hydrogen uptake apparatus

Br. Corros. J., 1967, Vol. 2, May


Booth et al.: Criteria of Soil Aggressiveness towards Buried Metals. I. 107

a fall of 0·8 pH units resulted from a change in the concen- 1 ml conc. hydrochloric acid and evaporated to dryness
tration of the slurry from 5 to 100 g soil per 50 ml water. again. The residue was dissolved in 20 ml distilled water,
Soluble iron concentration. The standard procedure adopted and the iron was determined colorimetrically with thio-
(using analytical grade reagents throughout) was to boil a glycollic acid.2 0 Results were expressed as parts per million-
sample of soil equivalent to 1 g dry weight with 50 ml dis- f-lg/g dry weight of soil. This test is rather too complex to
tilled water for 30 min. 5 ml of a saturated solution of incorporate in a 'simple' scheme for soil analysis, but was
potash alum was added to coagulate colloidal material, and included for general interest. Other quantitative chemical
the suspension was centrifuged at 8000 rev/min for 10 min. analyses were not attempted, mainly because of the special-
The supernatant solution was decanted and evaporated just to ised techniques required and because of the inconsistencies
dryness with 0·5 ml conc. nitric acid and 1 ml saturated previously encountered by Smith6 in attempts to correlate
potassium chlorate (to destroy organic matter), taken up in chemica1'composition of soils with their corrosiveness.

TABLE I
Results of aggressiveness tests on a soil
Name of site: Haverfordwest
Description of soil: Heavy, black, waterlogged and marshy soil
Corrosion history: Corrosion of pipelines recorded by Wales Gas Board
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'Bottle test',
Resistivity, Redox-potential, Water days to blacken Viable count of H2
pH Fe,
Q-cm at Vat pH = 7 content, sulphate-reducers, uptake,
p.g/g
3ft (N.H.E.) % Baars' Baars' medium cells/g ml
medium + cysteine
January 2,400 0·060 53 9 3 105 - 6·0 420
February 3,260 0·040 66 9 3 104 - 6·0 1000
March 1,630 0·040 59 9 2 106 - 6·1 104
April 2,300 0·070 52 5 6 104 - 5·9 250
May 2,010 -0·132 61 4 4 104 - 4·3 420
June 1,680 0·065 49 13 4 105 41 5·5 166
July 1,150 0·150 46 6 3 106 - 6·5 86
August 1,680 0·070 51 11 4 105 55 6·0 325
September 2,400 0·070 44 7 2 104 - 6·2 390
October 1,150 0·160 49 8 3 107 40 6·7 42
November 2,300 0·100 54 7 3 106 - 6·6 120
December 3,350 0·070 53 12 4 103 51 6·0 720

Mean 2,110 0·064 53 8 4 105 47 5·9 333

TABLE II
Results of aggressiveness tests on a soil
Name of site: Heston
Description of soil: Light brown loam with good crumb formation
Corrosion history: No incidence of corrosion reported by Metropolitan Water Board

'Bottle test',
Resistivity~ Redox-potential, Water days to blacken Viable count of H2
uptake, pH Fe,
Q- cm at Vat pH = 7 content, sulphate-reducers, p.g/g
3ft (N.H.E.) % Baars' Baars' medium cells/g rol
medium + cysteine
January 4,790 0·528 13 6 3 105 - 5·8 40
February 9,580 0·350 14 8 4 105 - 5·3 40
March 4,790 0·504 18 10 3 104 - 5·9 130
April 9,580 0·466 16 neg. 32 103 0 5·3 0
May 4,790 0·550 16 7 3 104 - 7·4 54
June 7,660 0·530 14 5 4 105 - 5·3 50
July 9,580 0·540 10 6 3 104 - 6·0 50
August 26,820 0·548 10 8 3 104 0 5·7 30
September 8,620 0·510 14 9 2 104 25 7·3 66
October 14,370 0·550 16 5 2 104 - 5·8 71
November 9,580 0·520 18 6 3 104 - 6·5 45
December 4,790 0·560 15 7 2 104 0 6·3 134

Mean 9,560 0·513 15 7 5 104 6 6·0 59

Br. Corros. J., 1967, Vol. 2, May


108 Booth et al.: Criteria of Soil Aggressiveness towards Buried Metals. I.
Results at the time that they were obtained. The use of mean values
Tables I and II show a complete set of results of the tests to develop a scheme for the prognosis of probable soil
as applied to two different .soils. Individual measurements aggressiveness, and the significance of individual test results
are tabulated according to the month in which they were are discussed in the second part of this report.
taken, but the measurements were spread over 5 years.
Even in just these two specimen tables most of the tests give
results having a considerable scatter about the mean. Acknowledgment
Occasionally, individual results diverge widely from the mean The work described above has been carried out as part of
but there is no indication that this is connected in any way the General Research Programme of the National Physical
with either the time of the year or with the weather prevailing Laboratory.

References
1. Butlin, K. R., & Vernon, W. H. J., J. Instn Wat. Engrs, 1949, 10. Starkey, R. L., & Wight, K. M., Am. Gas Ass. Monogr., 1945,
3,627 'Anaerobic Corrosion of Iron in Soils'
2. Correlating committee on cathodic protection, Corrosion, 1948, 11. Booth, G. H., Cooper, P. M., & Wakerley, D. S., Br. Corr. J.,
4,6 1966, 1, 345
3. Vernon, W. H. J., 'Conservation of natural resources', 1956, 12. Wenner, F., Bur. Stand. sci. Pap., 1916, No. 12, p. 469
p. 121 (London: Instn civ. Engrs) 13. Deuber, C. G., & Deuber, G. B., Am. Gas Ass. Rep., April 1956
4. Romanoff, M., Natn. Bur. Stand., Cire. 579, 1957 (Washington: 14. Hoar, T. P., & Farrer,T. W., Corros. Sci., 1961, 1,49
U.S. Govt Printing Office) . 15. Booth, G. H., Corros. Sci., 1962, 2, 227
5. Denison, I. A., & Ewing, S. P., Soil Sci., 1935, 40, 287
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16. Baars, J. K., Meinema N.V., W. D., Delft, 1930, Dissertation


6. Smith, W. T., West. Gas, 1931, (Feb.), p. 70 17. von Wolzogen Kiihr, C. A. H., & van der Vlugt, L. S., Water,
7. Tomashov, N. D., & Mikhailovsky, I. N., Dokl. Akad. Nauk 1934, 18, 147
SSSR, 1959, 124, 1285 18. Booth, G. H., & Tiller, A. K., Trans. Faraday Soc., 1960, 56,
8. Stratfull, R. F., Corrosion, 1961, 17, 493 1689
9. Tomashov, N. D., & Mikhailovsky, I. N., Corrosion, 1959, 19. Romanoff, M., J. Res. natn Bur. Stand., 1945, 34, 227
15,77 20. 'Methods of chemical analysis as applied to sewage and sewage
effluents', 1956, 2nd edn p. 79 (London: H.M.S.O.)

Br. Corros. J., 1967, Vol. 2, May

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