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Paper No. CORROSIONc)L

603 The NACE International Annual Conference and Exposition

TEMPERATURE AND VELOCITY EFFECTS IN NAPHTHENIC ACID CORROSION

H. Lee Craig, Jr.

Corro$ion Prevention & Control
1704 Havenwood Drive
Richmond, VA 23233

ABSTRACT

The effects of temperature and velocity were studied with respect to alloy selection for
corrosion resistant service. The amount of molybdenum in the austenitic stainless steel alloys
is critical in conferring corrosion resistance on the alloy as the temperature of the
environment increases. Velocity effects have been studied in a closed loop hot oil circuit
where the stream impinges on the target specimen. Film breakdown is prevented by
increasing the molybdenum content.

Keywords: Naphthenic Acid, Crude Oil, Laboratory Tests, Field Tests, Molybdenum-
bearing austenitic stainless steels.

INTRODUCTION

Austenitic stainless steel alloys containing molybdenum are used in those parts of refinery
equipment subject to naphthenic acid corrosion - usually in the vacuum distillation column,
heater and associated piping and exchangers. The attack may start at about 450 F (230 C),
reach a maximum around 750- 800 F (400 -430 C) and decrease somewhat above that
temperature range. The velocity of the process stream has a large impact on the observed
corrosion rate. Fractional distillation and consequent concentration of the acids in condensed
phases also produces accelerated attack. The desire to minimize capital investment in new
equipment, or in retrofitting older units has led to studies for assessing the corrosivity of
process streams and the sensitivity of corrosion resistance of alloys to changes in chemical
composition.

Copyright
@l996 by N,4CE International,Requests for perrn;ss;on to publlsh this manuscript in any form, in part or in whole must be made in writing to NACE
International, Conferences Division, PO. Box 218340, Houston, Texas 77218-8340. The material presented and the views expressed in this
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Laboratory experiments, coupled with field tests, are now being used to discriminate among
the various alloys proposed for combatting this corrosion problem. Piehl* conclusive y
demonstrated the requirement that an alloy, to be resistant at all to naphthenic acid, had to
contain at least 2 weight percent molybdenum. This is in addition to other elements which
provide high temperature sulfidation resistance, such as chromium. Relatively small
variations in alloying elements have been reported to affect corrosion resistance. Type 316L
stainless steel ( S3 1603) with a nominal molybdenum content of 2.0 to 3,0 %, but with
actually less than 2,5 % mol ybdenulm shows poorer corrosion resistance to naphthenic acid
attack than the same alloy with a molybdenum content on the higher side of the allowed
nominal range.

A better understanding of this phenomenon was sought by exposing a selection of alloys with
a range of molybdenum content in a hot oil test loop. The samples were used as targets of a
stream of hot oil, so as to determine their impingement resistance. Results from this
exposure test provide insight into the interaction of molybdenum content with temperature
and velocity effects.

EXPERIMENTAL PROCEDURE

Hot oil test loop

A system for circulating hot oil was built, incorporating a chamber in which a target
specimen was placed and against which a stream of the hot oi I was directed. Provision was
made for incorporating a control specimen in a relatively quiescent part of the test chamber,
so that the corrosivity due to temperature alone could be determined.

The conditions of testing were selected within the commonly accepted parameters for
naphthenic acid corrosion:z

PARAMETERS HOT OIL TEST LOOP CONDITIONS

TAN > 0.5 mg KOH/g oil TAN = 5, 10, 15, 20

Temperature 232 to 400 C (450 to 750 F) T = 232 C (450 F) or 370 C (700 F)

Test period (suitable for laboratory test) 72 hours

Flow conditions impingement, 100 to 450 ft/sec

Atmosphere (to prevent oxidation) Nitrogen

Coupon surface/oil volume ratio 50 sq cm/5 liters

The target specimen was a square plate, 5.0 x 5.0 cm (2-inch by 2-inch), 0.6 cm (0.25-inch)
thick. It was suspended under a carefully machined nozzle, which provided a stream of hot
oil, directed straight at the test surface.

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Because of the difficulty of maintaining the corrosive oil at elevated temperatures throughout
the test loop, the oil was circulated from a reservoir by a pump, through a heat exchanger,
and into the test chamber. After impinging on the specimen, the oil passed through coolers
before reentering the reservoir, where it was available for recirculation. While this concept
appeared simple, there were many experimental difficulties. Some of the oils tested were
prone to coking the heat exchanger. Naphthenic acids decompose when heated, producing
gas phases, such as carbon dioxide. Hydrogen sulfide gas is also produced by the thermal
decomposition of organic sulfur compounds in the oil. In order to follow the loss of acid
content over the period of the test, periodic samples were taken. Generally, these results
demonstrated that the decrease in acid content was minimal.

As a safety note, the entire apparatus was contained in a large, walkin test chamber, which
could be flooded with carbon dioxide should hot oil leak from the loop, and a fire start.

A preliminary test, utilizing a carbon steel target, was run to check out the operation. Some
data that was collected is shown in Table 1.

Table 1.

Oil properties for test run of 72 hrs at 700 F with a carbon steel target

Sample ID TAN Wt% s Viscosity - API - gravity

centistokes

HVGO-start 6.96 1.30 336.0 CS 14.9

HVGO-end 1.39 1.10 26.57 CS 14.5

Average 4.18 1.20

Upon removing the target coupon from the holder, it was observed to be heavily sulfided.
No erosion pattern was evident. It was concluded that the easily removed iron sulfide
coating protected the surface from highly selective attack, in a similar fashion as the heat
resistant tiles used on the space shuttle protect against thermal deterioration of the shuttle
skin, upon reentry. There was a loss of acid and, to a lesser extent, sulfur compounds, so
the decision was made, for subsequent tests, to add additional acids at the start to the test oil,
to compensate for the thermal decomposition of the acids. A commercially available mixture
of naphthenic acids was used to supplement the acids already present in the oil.

In the case of the control (quiescent) sample, (used in subsequent tests) a carbon steel coupon
was immersed in the sample of oil to be tested for its corrosivity. The uniform corrosion
rate, in mm/y (mpy) is measured by weight lost in the test, after the corrosion product film
has been carefully removed by bead blasting.

In order to study the effect of sulfidation corrosion, acting in concert with naphthenic acid

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corrosion, a modification in this approach was taken. The weight per unit area of corrosion
product film is determined by cleaning and drying the coupon after the test and weighing it
with the corrosion product intact. Then, the film is removed by bead blasting and the bare
coupon reweighed. The difference in weights is used to calculate the weight of corrosion
product which adheres to the metal after the test. A simple ratio of the corrosion rate, in
roils per year, to the weight of corrosion product film, in milligrams per square centimeter,
provides a “naphthenic acid corrosion index” (NAC1). s Briefly, this Index helps
discriminate among three forms of high temperature corrosion. If the value is less than 10,
the attack is mainly sulfidation. If the value ranges between 10 and 100, the attack is by
naphthenic acid, which is partially inhibited by the presence of hydrogen sulfide. Values
over 100 imply uninhibited naphthenic acid attack.

RESULTS

The first two test runs were designed to validate the equipment, i.e. to see if a distinction
could be drawn between two alloys which were expected to behave dissimilarly. The first
test employed as its target a sample of Type 3 16L stainless steel (2.4% Me), which is
known to be susceptible to localized corrosion in the naphthenic acids found in a West Coast
crude oil. The test was then repeated with a target of Type 317LS (S - special, 3.7% Me),
which is similar to the previous alloy, except that the molybdenum content is higher, by 1.3-
percent, than the Type 3 16L alloy sample.

The test conditions were maintained as similar as possible between the two runs. Because of
the loss of naphthenic acids during the trial, described above in the procedure section, a
deliberate addition of neat naphthenic acids was made to the starting oil, to try and make the
average acid content during the test period about a TAN of 5. A control sample of carbon
steel was included to measure the corrosivity under quiescent conditions. The results are in
Table 2.
Table 2.

Results of two impingement tests, run for 72 hrs at 700 F, using stainless steel(SS) targets

Conditions TAN Wt% s Corrosion rate, Impingement

CS, quiescent results - SS

Type 316L 9.15 1.10

start

end of test 1 3.69 1.00 72.9 mpy dimple

average 6.42 1.05

Type 317LS 9.95 1.00

start

end of test 2 0.44 0.98 133 mpy smooth

average 5.20 0.99

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In the case of the Type 3 16L sample, the “dimple” was a depression in the sample, opposite
the nozzle and about the same diameter as the impinging stream (1 mm). This provided
positive evidence that the conditions produced erosion corrosion, or impingement attack, on
this alloy. The Type 3 17L sample showed no effect of the impinging stream, other than a
thin coating of iron sulfide which apparently was suspended in the oil and had settled on the
specimen once the pump was shut off. It was easily wiped off.

This test was successful in demonstrating qualitatively the susceptibility to erosion corrosion
of the Type 3 16L alloy and the resistance of the 317LS to this type of attack, under closely
similar conditions. Even though the acid content fell off drastically in the second run, the
result obtained with the control specimen under quiescent conditions shows that the intrinsic
corrosivity of the oil was even greater for the second run than the first, despite the loss of
acid by the end of the test.

The next run (test 3) was an attempt to cause a failure in the Type 317LS, to try and judge
how close that material was to failing. It was also decided to take oil samples more
frequently during the run, to assess the rate of acid decomposition over the 72-hour period.
The results are in Table 3.

Table 3.

Impingement test results for Type 317LS at 700 F over 72-hour period for high acid content

Elapsed time TAN Wt%s corrosion rate Impingement

test 3 CS - quiescent results - SS

Start 12.42 1.05

10 hrs 10.06 1.04

30 hrs 5.59 0.96

37 hrs 4.85 0.93

55.5 hrs 4.09 0.94

72 hrs (end) 3.94 o,9~ 118 mpy slight etch

The sample surface showed only a slightly etched area opposite the nozzle, but no depth to
the attack. It was decided that this represented just the very beginnings of impingement
attack, probably occurring during the first 10 hours while the acid content was high.

The analyses for TAN showed that the acid decomposition fell exponentially and not linearly
over the test period. However, the value near the midpoint of the test, 4.85, is close to the
nominal 5.0 value typical of the gas oils under study, so that the test is considered typical for
that oil. The fact that a s]ight etch was found suggests that large amounts of acid may have a
corrosion effect on the alloy, but that its erosion resistance is still pretty good.

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The quiescent corrosion rate again validates the test, with regard to the corrosivity of the oil.

Tests at lower temperatures

In order to make a decision whether or not to replace some carbon steel piping at a crude
unit, two tests were run at the temperature of the light vacuum gas oil (LVGO) stream
handled by the piping, 450 F. The oil was made more corrosive by the addition of neat
naphthenic acids, since this process stream was projected to see an increase in acid content in
the future. The results are in Table 4.

Table 4.

Impingement test results for a light vacuum gas oil at 450 F in a 72-hour test period

Conditions TAN Wt%s corrosion rate Impingement

CS - quiescent results - SS

Carbon steel 11.09 1.54

start of test 4

after 24 hrs 11.08 1.41

after 48 hrs 11.00 1.46

end -72 hrs 11.07 1.48 37.1 mpy film effect only

Type 316L

start of test 5 24.65 1.32

after 24 hrs 24.74 1.25

after 48 hrs 24.70 1.30

end -72 hrs 24.64 1.37 45.6 slight etch

Carbon steel developed a circular pattern in the iron sulfide film, but no significant attack on
the underlying metal. The Type 3 16L sample showed the same kind of acid etch that the
Type 317LS had developed previously, in the presence of high concentrations of acid, as
shown by the TAN values.

These two tests confirmed earlier results, regarding the effect of temperature. This lower
temperature activates naphthenic acids only slightly, even when the concentration is high.
Also, the lower temperature does not cause decomposition of the acid.

A standard laboratory test was run at 500 F on a sample of the LVGO that had not been

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doped. The TAN was 3.53 and the corrosion rate was 9.6 mpy, which represents a
reasonable corrosion rate for carbon steel due to sulfidation at this temperature, without any
great impact by the naphthenic acid.

Note that neither the naphthenic acids nor the organic sulfur compounds show a tendency to
decompose at this temperature. Although the second run has considerably more acid in it
than the first one, the corrosivity towards carbon steel is not greatly enhanced and the
stainless steel is only slightly affected.

Effect of Velocity - field observations

Due to the limited erosion seen in these laboratory tests, no conclusions about the effect of
velocity were drawn, other than the “pass-fail” type of assessment given in the tables. These
tests were carried out four years ago (199 1). Since then, there have been no incidents
involving erosion corrosion at the refinery on whose behalf the tests were performed.
Inspection during the latest turnaround (1993) showed that the piping, heat exchangers,
pumps and sections of the vacuum column fabricated from Type 3 17LS have withstood the
corrosive service very well. In the past, frequent repair or replacement of Type 3 16L or
lower alloy equipment and linings was routine during turnarounds.

Effect of Temperature - static tests

In addition to the velocity, the temperature of the attack has a great influence on the
corrosion rate. High temperatures appear to activate even comparative y small amounts of
naphthenic acids in the oil. This has been demonstrated in the laboratory, while studying
alloy selection and inhibition of certain process streams. For example, in a series of tests
with samples of process streams from a South American (SA) crude oil, and a comparison
sample from Australia, the following results were obtained, as shown in Table 5.

Table 5.

Laboratory Corrosion Tests on Carbon Steel

Test Temp (F) VTB - Austr. AGO - SA LVGO - SA HVGO - SA

TAN = 0.82 TAN = 1.93 TAN = 3.47 TAN = 2.80

mpy NAC1 mpy NAC1 mpy NACI mpy NAC1

500 0,6 6.1 4.1 10.3 -

600 7.5 6.1 -

650 44.0 19 -
172 20 280 21.1 320 44.6
700 -
I
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This series established the corrosivity of the two vacuum gas oils at 700 F. At the same
time, a series was run with Type 3 16L stainless steel, to determine the suitability of that
alloy for equipment to be used in this service, as shown in Table 6.

Table 6.

Laboratory Corrosion Tests of Type 3 16L Stainless Steel

Test Temp F VTB - Austr. AGO - SA LVGO - SA HVGO - SA

mpy nlp y mpy mpy

500 0.3
700 4.7 8.8 12.8

These corrosion rates suggested that an even higher alloy, such as Type 317L, would be
preferred for service in this equipment, rather than Type 316L, which these results represent.

Effect of Temperature - Inhibitor tests

A similar pattern of behavior was found when a process stream was tested during a program
to check the efficiency of inhibitors. This stream was the feed to the vacuum distillation
system, from the bottom of the atmospheric distillation column, called “atmospheric tower
bottoms (ATB, TAN = 0.86)”. The standard laboratory test was run, except that the
temperature range covered the expected temperatures in the unit. The results are in Table 7.

Table 7.

Naphthenic Acid Corrosion Tests - Carbon steel in ATB

Test Temperature Corrosion Rate, mpy NACI

500 F (260 C) 0.3, 0.9 4.6,6.1

600 F (316C) 10.9, 9.9 7.0,6.6

700 F (371 C) 95.0, 101.6 18.2, 22.7

u

The corrosion rate increases with temperature, as expected. The rates at 500 F (260 C) are
exceptionally low, probably due to the fiact that the oil has been heated well above that
temperature, decomposing reactive sulfur compounds and some of the naphthenic acids. Up
to 600 F (316 C), the corrosion is predominantly sulfidation. At 700 F (371 C), the

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sulfidation is aggravated somewhat by naphthenic acid, although this is not a severe case of
naphthenic acid corrosion, as shown by the moderate values of the NAC1.

Once the above base line was established, tests were run at 700 F (371 F) using the inhibitor
currently in service on that unit. The results are in Table 8.

Table 8.

Naphthenic Acid Corrosion Inhibitor Tests - Carbon Steel, Inhibitor A, 700 F

Concentration, ppm Corrosion Rate, NAC1 Efficiency, %

mpy

10 autoclave leaked -

50 74.8 4.2 24

200 28.2 21.5 71

L-

The most important parameter to look at here is the drop in corrosion rate and the increase in
efficiency, as the concentration of inhibitor increased. The NACI may include a component
due to protective film formation, and may not be a reliable index of type of attack in the
presence of a film forming inhibitor. Interval tests over longer periods would have to be
carried out to determine this factor. Efficiency is calculated by subtracting the inhibited
corrosion rate from the uninhibited rate (Table 7), dividing this by the uninhibited rate and
multiplying by 100 for the percentage figure.

Due to the difficulty of maintaining the seal in the autoclave when the entire vessel is in the
furnace, heating mantles were employed for subsequent tests. Therefore, the control (no
inhibitor) case was repeated, and efficiencies given in Table 9, below, are calculated based
on the value for this sample.

Table 9.

Inhibitor tests at 50 and 100 ppm concentration

Test Corrosion rate, mpy NACI Efficiency, %

ATB (control) 36.5 18.7

Inh. A -50 ppm 27.5 13.9 25

Inh. B - 50 ppm 16.4 12.8 55

Inh. C - 50 ppm 23.4 14.2 36

Inh. C - 100 ppm 16.2 6.8 56

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The testing of these inhibitors was performed under slightly different conditions, using a
heating mantle for the autoclave instead of putting the autoclave in the furnace. This resulted
in a slightly lower temperature for the test, even though the controller was set for 700 F, due
to heat losses through the top of the autoclave, which was not insulated. It was concluded
that there was little difference in these tests among inhibitors, and that field trials should be
carried out to determine effective dosages and costs.

DISCUSSION

Carbon steel and the austenitic stainless steels tested in this work all are protected from
corrosion by naphthenic acid by a film which forms on the surface at the temperature of the
test. This film is composed of iron sulfide in the case of carbon steel. Austenitic stainlesses
form complex films which contain the alloying elements present in the base metal. Erosion
corrosion of the metal takes place by a film removal mechanism, whereby, once the
protective fi hn is removed by the impinging stream, the metal dissolves as it attempts to
reform the film. The alloy components form oil soluble salts, such as iron naphthenate, so
that protective deposits of corrosion product are not allowed to build up on the surface. This
mechanism was evident in all the tests described above.

However, in some cases, a somewhat protective iron ( or iron-chrome-moly) sulfide film

may be left on the surface. This phenomenon has led to the classification of naphthenic acid
corrosion into three types:

Type I - pure naphthenic acid corrosion - sulfur compounds have little or no

effect, if they are present

Type 11- Sulfidation corrosion, accelerated by the presence of naphthenic acids

Type 111- Naphthenic acid corrosion, inhibited by hydrogen sulfide

Figure 1 shows the laboratory data on which this classification rests. The upper, heavy solid
line represents Type I corrosion, which produces a relatively film-free surface and very high
corrosion rates in the metal. The lighter, “ess-shaped” curve demonstrates the difference
between Type 11 and Type Ill attack. The lower corrosion rates at the left hand side of the
curve represent heavily sulfided metal, in which the film is beginning to deteriorate, but is
still largely protective - this is Type 11attack, sulfidation accelerated by the presence of
small amounts of naphthenic acid. The higher corrosion rates at the right hand side of the
curve are produced when only very little of the protective film remains, but the acid attack is
slowed, probably by the suppression of ionization by the stronger acid (hydrogen sulfide).
These results (upper curve) were obtained with a neutral, sulfur free oil to which naphthenic
acid was added. For the lower curve, hydrogen sulfide gas was also added to the oil where
the effect of that acid was being determined. ~

The four asterisks represent corrosion data for carbon steel in a sample of heavy vacuum gas

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oil(HVGO) obtained from the retlnery. This oi I contains organic sulfur compounds,which,
when heated, decompose to form hydrogen sulfide. Carbon steel exposed to hot HVGO
forms a protective iron sulfide film, as a rule. The corrosion rate data was obtained using
the same test as was used for the neutral oil, doped with commercial naphthenic acid. The
difference between the corrosion mechanism for these sulfur free oils and the HVGO is that
the corrosion rates are reduced due to the somewhat protective nature of the film.

The hourglass symbols represent two HVGO samples, doped with commercial naphthenic
acid and taken before the loop tests began. The corrosion tests reported here were also
performed at 500 F, the “standard” test temperature used for comparing the corrosivity of
various oils. Although no analyses were performed for the amount of hydrogen sulfide in
the oils, it is suggestive by the results that sufficient reactive sulfur compounds were present
to suppress the activity of the acid by one means or another (film formation or suppressed
ionization).

The two diamond-shaped points represent corrosivity measurements under standard

conditions (500 F, 48 hours, autoclave) for carbon steel coupons tested in HVGO samples,
obtained after the hot oil loop impingement corrosion test was completed. The acid content
had decreased in each case, which lowered the corrosion rates found in these oils. Exposure
to temperatures up to 700 F in the loop test also reduced the amount of sulfide film-forming
components, so that these results are quite similar to the neutral oil, doped with acid.

CONCLUS1ONS

A hot oil loop laboratory test for naphthenic acid corrosivity has proven useful in
selecting materials of construction for equipment subjected to corrosion by oils bearing
naphthenic acids as well as sulfur species. The test may be run at temperatures of interest
using samples of the process streams in question, or closely related oils. It is an
impingement test, performed under conditions designed to investigate the influence of high
flow rates.

The influence of molybdenum as an alloying element in austenitic stainless steels and

related alloys has been further defined. Under impingement conditions, in the presence of
high concentrations of acid, as in certain zones within a vacuum distillation tower, alloys
with insufficient molybdenum may suffer film breakdown and accelerated corrosion. A 1.3-
percent increase in molybdenum content appears to increase the corrosion resistance of this
class of alloys sufficiently to withstand impingement by hot oil containing typical amounts of
naphthenic acid, with TAN values in the range of 6 to 10. For furnace tubes and vacuum
tower internal structures, the higher molybdenum-bearing alloys will provide the more
corrosion resistant behavior.

A measure of naphthetlic acid corrosivity, called the, “naphthenic acid corrosion

index” (NACI) is a simply obtained numerical factor which separates naphthenic acid
corrosion, sulfidation affected by naphthenic acid corrosion, and simple sulfidation attack.
This index is the ratio of the corrosion rate in roils per year to the weight of adherent

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corrosion fihn deposit in milligrams per square centimeter. Values under 10 imply that the
corrosion is largely sulfidation. Greater values suggest increasing naphthenic acid attack.

The limitations of using the ru]e-ot-thumb that naphthenic acid-bearing oils are only
corrosive if the TAN exceeds a value of 0.5 have been shown to be due to the effect of
temperature in activating even small concentrations of acid in certain oils, as well as the lack
of correlation between TAN and any rigorous measure of corrosion.

The generally accepted influences of temperature, velocity and concentration of acid

by fractional distillation have again been demonstrated.

ACKNOWLEDGEMENTS

The author would like to acknowledge the careful laboratory work of David S.
Hampton and David H. George. The cooperation of several Mobil Oil coworkers is also
gratefully acknowledged: Gary Rusk, Fu Hwang , Joe Sodomin.

The hot oil test loop was designed, constructed and operated by Cortest Laboratories, Inc.,
Houston, TX. The input by Russ Kane, Mark Wilhelm, Bob Asperger, Bernie Ramirez and
several others of the staff is acknowledged.

REFERENCES

1. R. L. Piehl, “Naphdlenic Acid Corrosion in Crude Distillation Units”, Corrosion/87,

paper no. 196, (Houston, TX: NACE, 1987) Table 5, page 196/10

2, E. Babaian-Kibala, H. L. Craig, G. L. Rusk, K. V. Blanchard, T. J. Rose, B. L.

Uehlein, R. C. Quinter and M. A. Summers, “Naphthenic Acid Corrosion in a Refinery
Setting”, Corrosion/93, paper no. 631, (Houston, TX: NACE, 1993), page 631/3

3. H. L Craig, “Naphthenic Acid Corrosion in the Refinery”, Corrosion/95, paper no.

333, (Houston, TX NACE, 1995)

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Figure1 - Naphthenic Acid Corrosion
Effect of Hydrogen Sulfide

Corrosion Rate (mpy)

50

5
024 6810121416182022 24
TAN

— K1 + H2S — Acid (Kl)

,,” ~
~.
/’ HVGO - AT HVGO+Acid

HLC - 8/9/95 - EFFH2S