Beruflich Dokumente
Kultur Dokumente
Abstract
This section covers materials of construction and other controls used to minimize
corrosion in furnace tubes and transfer lines, atmospheric and vacuum columns,
column overhead systems, and other crude distillation facilities. Corrosive agents
include high-temperature H2S, naphthenic acids, and HCl.
Contents
Page
3100-3
3100-9
3100-18
3100-21
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August 1999
3100-28
3100-29
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3100-31
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0.5 to 2%
Middle East
1 to 3%
Africa
0.2 to 1%
Venezuela
1 to 5%
Inorganic Salts
As received by the refineries, all crude oils contain some quantity of inorganic salts,
such as chlorides of sodium, magnesium, and calcium, sulfates, and carbonates.
While these salts are sometimes found as distinct crystals in the crude, they most
commonly occur in aqueous solution, having dissolved in the water accompanying
the crude. The salt content of crude oils may vary from 2 pounds to 200 pounds per
thousand barrels (PTB), but as received by refineries most crudes contain less than
30 PTB. Crudes shipped over the water in tankers generally average 1015 PTB
higher in salt content than those transported by pipeline.
Organic Acids
Various types of organic acids are found in crude oils. In the case of a few crudes,
they may exist in quantities large enough to constitute a serious corrosion problem
during processing. Of these, naphthenic acids are the most common. Crude oils
containing large quantities of naphthenic acid come from many locations, including
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Sulfur Corrosion
Hydrogen sulfide is corrosive to carbon steel at temperatures above 500F and may
also contribute to corrosion and/or stress corrosion cracking at lower temperatures
in the presence of liquid water. Since most crudes contain little dissolved hydrogen
sulfide, it might be concluded that corrosion due to sulfur compounds should not be
particularly serious in crude distillation units. Unfortunately, many of the commonly
occurring sulfur compounds thermally decompose on heating to liberate hydrogen
sulfide. It is this liberated H2S that is responsible for most high temperature crude
unit corrosion in the form of high temperature H2S corrosion (also called
sulfidation). [1]
High Temperature H2S Corrosion (Sulfidation). The degree to which the sulfur
compounds of various crudes decompose to liberate hydrogen sulfide is shown in
Figure 3100-2. These data were obtained by a laboratory test involving heating the
crude sample at a controlled rate and measuring the quantity of hydrogen sulfide
evolved as a function of temperature. It is obvious from these curves that the
different varieties of crude oil vary significantly in the rate at which hydrogen
sulfide is evolved. While not apparent from the data, different crudes from the same
general area may differ widely in H2S evolution characteristics. This is particularly
true in the case of Arabian crudes. Imported crudes, as received at domestic
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refineries, may also vary in hydrogen sulfide evolution as a function of their having
been stabilized prior to shipment.
Fig. 3100-2 Hydrogen Sulfide Evolution from Crude Oils, Chevron Proprietary Test Data
Since hydrogen sulfide is responsible for nearly all of the corrosion caused by sulfur
compounds, it is possible to obtain some measure of the corrosivity of a crude
oil by evaluating its tendency to evolve H2S upon being heated. For example,
Figure 3100-2 suggests that Santa Maria crude would be far more corrosive at any
temperature than Kettleman Waxy, and anyone familiar with the processing of these
two crudes would agree.
It is important to recognize that the hydrogen sulfide evolution test is a far better
criterion of corrosivity than the sulfur content of the crude. Because sulfur
compounds differ widely in resistance to thermal decomposition, it is not unusual to
find high sulfur crudes that are less corrosive than crudes containing only a fraction
as much sulfur. Results of hydrogen sulfide evolution tests on specific crudes may
be obtained from CRTC Materials and Equipment Engineering if an interpretation
of significance is desired; otherwise, directly from CRTC Process Planning.
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Wet H2S Cracking. At lower temperatures, where liquid water is present, wet H 2S
cracking is a potential concern. In crude units, such cracking is possible in the
column overhead and light ends systems. Refer to Section 450 of the Corrosion
Prevention and Metallurgy Manual for guidelines on addressing wet H2S cracking
concerns.
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commonly used test. The test estimates two values: total acid number (TAN) and
strong acid number. The neutralization number is the total acid number minus the
strong acid number. As most crudes do not contain strong acid, the TAN is often
equivalent to the neutralization number.
Naphthenic acids cause corrosion because they convert normally protective iron
sulfide into oil-soluble iron naphthenate. The acid may dissolve the iron sulfide
scale entirely or only partially, leaving a poorly adherent material which is readily
stripped off by high velocities or turbulence. There is a competition between H2S
forming the scale and naphthenic acid dissolving it. At high neut numbers, any
sulfide scale present is dissolved and corrosion occurs. See References [5], [6], and
[7] for an in-depth discussion of naphthenic acid corrosion.
As may be expected with any corrosive constituent, the degree of corrosion encountered with naphthenic acids will be higher in those areas where the acid is allowed
to concentrate. In a crude unit, the areas of most severe naphthenic acid corrosion
are usually in those parts of the columns (particularly the vacuum column) where
the acids become concentrated by distillation.
The potential for naphthenic acid corrosion is largely dependent on neut number
(processing crudes with high neut numbers results in more corrosion). Previously
published thresholds for corrosion were reliable for California crudes, but recent
experience has shown the threshold may be different for other crudes.
Some general guidelines are as follows:
At low velocities, corrosion with California crudes has not been significant if
the neut number for the hydrocarbon fraction is below 1.5 mg/gm.
At high velocities (>100fps, like transfer lines, furnace tube return bends, outlet
headers), corrosion has been observed at neut numbers as low as 0.3 mg/gm.
These neut number thresholds do not hold true for all crudes. Some recent
examples of corrosion are:
In conclusion, we are still learning more about naphthenic acid corrosion. If you are
processing a crude with no previous experience, contact CRTC Materials and
Equipment Engineering for up-to-date advice. Assume that a crude with any naphthenic acid is potentially corrosive.
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A phosphorus-based corrosion inhibitor is being used on a trial basis at Pascagoula. Along with determining its effectiveness against naphthenic acid corrosion, the effect of phosphorus on fixed bed catalyst will be monitored. Contact
Materials and Equipment Engineering at CRTC for more information.
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Neutralize
Yes (NH3,
neutralizing
amines)
Wash water
recirculation
also important
Inhibit
Magnesium chloride
and calcium chloride
decompose on heating
to form HCl
Monel
Cupro-Nickel
Admiralty
Carbon Steel
300 Series SS
12% Cr
9% Cr
7% Cr
5% Cr
Carbon Steel
No
No
No
On trial basis at
Pascagoula. Contact
MEEU for current
information.
Salts
(HCl)
Sulfur
Compounds
(H2S)
Naphthenic
Acids
Upgrade Alloy
(Best to Worst)
Where Corrosion
Occurs
No
Atmospheric
Column
Vacuum
Column
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Fig. 3100-5 Typical Areas in Crude Units Susceptible to Naphthenic Acid Corrosion
Atmospheric
Column
Vacuum
Column
Atmospheric
Column
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Vacuum
Column
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crudes on which both corrosion and H2S evolution data are given, a direct relationship exists between these two variables. A quantitative relationship between H2S
evolution, temperature, and corrosion rate is given in Figure 3100-8. At the H2S
levels typically found in crude units, metal temperature is the most important variable affecting corrosion.
While the corrosion data in Figures 3100-7 and 3100-8 are correlated with stock
temperature, the actual rate of attack on furnace tubes is greatly influenced by the
temperature of the tube wall. As might be expected from the corrosion rate curves,
attack on furnace tubes is highly dependent on temperature distribution in the
furnace. It is not unusual to find accelerated attack at hot spots on tubes, and a high
eccentricity factor resulting from preferential corrosion on the fired side of the tube,
as shown in Figure 3100-9. It does not necessarily require extreme localized overheating to create a situation in which essentially all of the corrosion occurs on the
fired side of a radiant tube. As a rule of thumb, furnace tube corrosion rates double
for each 35F to 40F increase in temperature.
Fig. 3100-7 Corrosion of Carbon Steel Furnace Tubes by Various Crude Oils
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Fig. 3100-9 Furnace Tube Failure as the Result of Preferential Corrosion on the Fired Side
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Fig. 3100-10 Furnace Tube Corrosion by Crudes Containing Naphthenic Acids and
Evolving H2S
noted here that naphthenic acid corrosion is a liquid phase phenomenon. In a twophase system, it is the liquid phase that is corrosive. Corrosion can also occur in the
vapor if mist or liquid droplets are present.
Some crude units require higher alloys than the 5-9% Cr steels for furnace tubes
when processing the very highly naphthenic crudes like SJV. Better materials, in
order of increasing corrosion resistance, are the 18-8 stainless steels (Types 304,
304L, 347), 16-13-3 Cr-Ni-Mo stainless (316 and 316L), the slightly higher alloyed
317 and 317L Cr-Ni-Mo stainless steels, and Inconel 625. The exact service limits
for these materials, in terms of temperature and neutralization number, have not yet
been established. Choice of furnace tube materials for high-naphthenic service is
best made after reviewing field experience of various materials in the most similar
crude service.
When selecting stainless steel furnace tube materials, the possibility of polythionic
acid stress corrosion cracking should also be considered. See the Corrosion Prevention and Metallurgy Manual, Volume 1, Section 400 for a detailed discussion of this
phenomenon. When considering both naphthenic and polythionic attack at the same
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Fig. 3100-11 Effect of Naphthenic Acid Corrosion on a Carbon Steel Furnace Tube
time, Type 347 stainless may be adequate if naphthenic acid corrosion is mild; this
alloy has the best resistance to sensitization and polythionic acid attack. If a
molybdenum-containing grade is needed for naphthenic resistance, use Type 316L
(2.5% Mo min) or 317L. These materials may sensitize in time. To avoid eventual
polythionic attack, it is important to minimize the tubes exposure to water and
oxygen. In some cases, plants utilize a carbonate wash procedure and dehumidifiers
during the shutdown process.
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When low-carbon grades of stainless steel such as 316L and 317L are used for
transfer lines, the possibility of their sensitizing in service must be considered. If the
line operates above about 700F, sensitization is likely and limiting contact with air
and water is critical. If the line must be opened to the atmosphere, carbonate
washing is desirable to minimize the chance of polythionic acid cracking.
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Fig. 3100-12 Typical H2S Corrosion Rates Above the Flash Zone in Crude Columns
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sulfur compounds in the oil continuing to decompose and liberate fresh hydrogen
sulfide. Where this has occurred, it is typically found that the bottom head corrodes
more rapidly than the column shell in the stripping section area. H2S corrosion can
also occur on the reduced crude side of bottoms exchangers.
It is interesting that the corrosion rates in the flash zone may be increased significantly with any given crude by increasing the outlet temperature of the atmospheric
furnace. This results in a higher flash zone temperature, as well as an increase in
evolved H2S. A secondary result is that because of higher H2S concentrations the
rate of corrosion within the entire column will be raised.
The relative order of corrosion resistance of various alloys in the atmospheric
column is also important. While carbon steel is subject to corrosion in varying
degrees in the flash zone area, it usually has adequate resistance in most other areas
of the column. The chromium steels and chrome-nickel stainless steels are usually
good. Trays and strip lining of 12% Cr steel are necessary above the flash zone
when processing crudes such as Arabian Light which evolve high amounts of H2S.
Nonferrous materials such as Monel and the copper-base alloys will be severely
corroded in any part of the column where temperatures exceed about 500F.
Historically, little naphthenic acid corrosion has been experienced in atmospheric
columns. But some danger of naphthenic acid attack may exist in the atmospheric
columns of single stage crude units. Conditions favoring its occurrence are highly
naphthenic crude feeds, and high transfer line temperatures (over 700F). Under
these conditions, the hottest sidecuts could contain enough naphthenic acids to be
corrosive. Naphthenic acid corrosion is covered in Section 3132.
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naphthenic acid corrosion may ultimately require alloy protection throughout the
column.
Unlike the atmospheric column, the vacuum column itself may be subject to severe
naphthenic acid attack when highly naphthenic crudes are being processed. Such
corrosion is typified by sharp-edged channels and grooves in areas of high fluid
velocity and the absence of corrosion products (because most metal naphthenates
are oil-soluble). Packing is particularly susceptible. Company units have seen structured packing corrode in columns where sidecut neut numbers were believed to be
well below 1.5.
For crude oils high in naphthenic acid, it is necessary in most cases to protect the
vacuum column with Type 316L (> 2.5% Mo) or 317L stainless steel. The extent of
protection depends on the distribution of naphthenic acids within the column.
Alloys less expensive than Type 316L stainless steel, such as Types 304L, 321, and
347 are an improvement over carbon steel in such environments, but usually do not
provide long enough lives.
Company experience has shown that naphthenic acid corrosion is seldom significant below about 350F. At higher temperatures, naphthenic acid attack may be
expected if the neutralization number of the sidecut stream exceeds 1.5 mg potassium hydroxide (KOH) per gram.
On rare occasions, vacuum column top heads have suffered corrosion at temperatures above the boiling point of water but below 350F. This temperature range is
too high for hydrochloric acid corrosion, and too low for naphthenic acid attack.
Although this corrosion has occurred in plants processing naphthenic crudes, the
appearance of corrosion is smooth, unlike typical naphthenic acid corrosion. The
best current theory is that such corrosion is due to other acidic organic compounds,
like phenols, and is possibly accelerated by the presence of chlorides [6]. When this
type of corrosion is encountered, the remedy has been to line the affected areas with
Type 316L stainless. Neutralization is not an effective remedial measure.
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system, carbon steel corrosion control simply requires adequate water recycle and
pH levels above the threshold for carbon steel corrosion.
Without saturation water recycle, corrosion control is exceedingly complex.
Although other corrosion control methods such as desalting and/or caustic injection
are often used along with wash water recirculation, these methods become even
more important if water recycle is not used. Also, alloy tubes are usually required
for the initial condensate and water reboiling region. If copper based tubes are used,
two sided pH control is needed to avoid corrosion of the copper alloy at high pH
and the carbon steel and copper components at low pH.
In general, this approach to corrosion control follows the Crude Unit Atmospheric
Overhead Corrosion Control Best Practice [8]. Although the Best Practices
approach differs from the rest of the industry, Chevron has successfully designed
and operated crude unit overheads with this philosophy since the early 1970s.
Specific Corrosives
Due to both the use of stripping steam in the atmospheric column and the presence
of water in the crude feed, large quantities of moisture are invariably present in the
atmospheric column. This moisture is, for the most part, condensed in the atmospheric column overhead-feed exchangers and overhead condensers. Where vapor
line temperatures are low (on the order of 200F), water may also condense in the
top of the atmospheric column. As a result, corrosion problems caused by liquid
water will be found throughout this area. For simplicity, the following discussion
includes the top few trays of the atmospheric column.
As mentioned, chloride salts in the crude oil form hydrochloric acid at elevated
temperatures by hydrolysis. This reaction occurs during heating of both atmospheric and vacuum column feed streams. The acid thus formed enters atmospheric
and vacuum columns and eventually leaves with the overhead product. Since HCl is
water-soluble, it is absorbed in any moisture that may condense, forming a strongly
acidic solution. While there is no evidence that HCl has any corrosive effect in the
crude distillation unit in the absence of liquid water, aqueous hydrochloric acid
solutions are the primary cause of corrosion in the overhead system, where liquid
water normally exists. Corrosion can also occur in the top part of the atmospheric
column, if liquid water exists.
Although not the primary corrosive, hydrogen sulfide also contributes to overhead
system corrosion. The usual corrosion products formed in overhead equipment are
iron and copper sulfides (on steel and copper alloys respectively). Metal sulfides
will either be stable or unstable (they will form or dissolve), depending on pH in the
system. Both iron sulfide and copper sulfide dissolve at low pH while copper sulfide
also dissolves at high pH. This is a fundamental reason why acid conditions (low
pH) corrode both copper alloys and steel, while alkaline conditions (high pH)
corrode copper alloys.
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3143 Desalting
The first place in the crude unit process flow where overhead corrosion can be influenced is in the desalter. Both chemical and electrical desalting are used in Chevron
crude units. It is important that the desalter provide a consistently low salt content.
A variable salt content introduces a control problem, because changing amounts of
HCl result in pH swings in the overhead system. Monitoring of pH and controlling it
by constantly varying the rate of neutralizer injection then becomes very difficult.
Recovered oil can be an important cause of pH instability. From the corrosion engineers view point, the recovered oil should be added to the crude as far upstream as
possible to facilitate removal in the desalter. If it is fed directly to the atmospheric
column because of heat exchanger and furnace fouling concerns, recovered oil
raises the average amount and variability of chlorides going overhead. Any sources
of increased or fluctuating chloride levels increase the difficulty of controlling overhead pH and corrosion.
Chevron Corporation
Concentrated caustic can cause stress corrosion cracking and general corrosion
of piping and exchangers downstream of the injection point.
Caustic can cause furnace fouling. This phenomenon has not been seen in crude
furnaces, but it has occurred in coker furnaces.
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Caustic can cause unacceptable sodium carryover in the coke produced in coker
units.
Risks of stress corrosion cracking and corrosion can be mitigated by utilizing the
Caustic Injection Facilities Standard Design [2]. Where crude unit residuum is fed
to a coker or a catalytic process, such as an RDS, the risks to the catalyst must be
studied before injecting caustic in the crude unit.
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Chevron Corporation
3146 Neutralization
No matter how effective desalting and caustic injection may be, some hydrogen
chloride (HCl) will always be evolved when the crude is heated. Being volatile, the
HCl will go overhead in the atmospheric and (to a lesser extent) the vacuum
columns. It will be absorbed in the condensing water, where it will form a hydrochloric acid solution. This acid is so corrosive that without process control countermeasures, corrosion prevention would require the use of expensive alloys such as
Hastelloy B or Hastelloy C. Water recirculation dilutes the acid, but neutralization is
required to raise the pH. The industry has adopted the practice of neutralizing the
acid by injecting either ammonia or a neutralizing amine into the overhead system.
The Company Best Practice is to use aqueous ammonia as the neutralizer, unless a
plants specific design and operation limit its effectiveness. If questions about the
appropriate neutralizer arise, consult with a Company Materials Engineer. The
choice should not be left to chemical suppliers, who may overemphasize the benefits of their chemicals and downplay the disadvantages.
Ammonia
Ammonia is an excellent neutralizer, is readily available, is relatively inexpensive,
and causes no downstream fouling problems. In the aqueous form it is also convenient and easily controlled. Anhydrous ammonia is not recommended because injection rates are hard to control and greatly influenced by atmospheric temperature
changes.
Anhydrous or aqueous ammonia can be purchased, but they should be diluted to a
10 wt % solution before injection into the crude unit overhead. Dilution water
should contain no more that 25 ppm of total dissolved solids in order to prevent
deposition in the overhead system. The ammonia should be injected into a sidecut
stripper vapor return line or (preferably) into the column overhead vapor line
through an injection nozzle and reliable pumping system. An accurate and reliable
measurement of ammonia flow rates is also important for maintaining system
control. Design recommendations are further detailed in the CRTC document
Design Recommendations Aqueous Ammonia System Corrosion Control Crude
Until Overhead Systems. [3]
If water injection is sufficient to achieve saturation, evaporation ceases and
ammonia neutralization becomes effective. As the vapors pass through the overhead system and are cooled, increasing amounts of condensing water remain as
liquid. HCl and neutralizer are absorbed at different rates. In an HCl/NH3 system,
the HCl is absorbed more rapidly, so the initial liquid is relatively acidic. As
condensation proceeds, more ammonia is absorbed in the liquid and the pH rises.
Corrosion continues wherever low pH water is present.
Unfortunately if water injection is insufficient, corrosive ammonium chloride
deposits can form. As condensing water has a dew point, condensing ammonium
chloride has a sublimation point. Depending on the conditions in the plant, either
ammonium chloride or water may condense first. If water condenses first, the
ammonium chloride dissolves in the water and no salt deposits form. If ammonium
chloride condenses first (sublimes), salt deposits form. When ammonium chloride
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salts deposit on colder surfaces, water vapor permeates the deposit and condenses
on the surface. The resulting aqueous ammonium chloride film is highly corrosive
and causes pitting.
Neutralizing Amines
Chemical vendors have long advocated the use of neutralizing amine rather than
ammonia for overhead pH control. They claim that using amines prevents the low
pH in the initial water condensate which is ascribed to ammonia. They fail to point
out these disadvantages, however:
Their high cost prohibits using enough to raise the pH to an optimal level.
Neutralizing amines and their reaction products can cause fouling, corrosion,
and carry chlorides into downstream processes.
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corrosive constituents and the metal. These high molecular weight, organic liquids
have some affinity for both oil and water. They are non-volatile, so they are not
present in the vapor phase.
Since the water phase in overhead systems causes the corrosion, a filming amine
that has a preferential affinity for water would be a likely choice for corrosion
prevention. However, these filming amines are washed away by flowing water,
especially in high velocity areas, and do not provide adequate protection. Filming
amines that have a preferential affinity for oil often do not reach the surfaces that
are water wetted, so they also fail to protect. In addition, any dead areas in the
system that are not liquid wetted will not be protected by the non-volatile filmers
when condensation and evaporation occur.
Besides their lack of effectiveness, filming amines can actually create problems.
Concentrated filmers may be corrosive. If they are not carefully diluted and
injected, they will corrode carbon steel. Inhibitors can cause fouling. They can leave
gummy deposits in instrumentation, reboilers, and heat exchangers in downstream
equipment.
A final and compelling argument against using inhibitors is that they may not be
necessary. If both overhead system design and corrosion control program are good,
corrosion rates will be low enough to make an inhibitor unnecessary. Although
chemical vendors may disagree, there is no justification for spending money on
filming amines in crude unit overheads.
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Atmospheric overhead vapor lines are constructed of carbon steel. Typically, corrosion is more moderate and alloys such as Monel are seldom justified. However,
some potential for corrosion exists here, and vapor lines should be routinely
inspected by ultrasonic and/or radiographic techniques, particularly at bends and
just downstream of bends and at injection points.
August 1999
Maintain all chemical injection pumps, flow meters, and instrumentation so that
the system is a reliable, continuous ammonia (or caustic) source.
Ultimately the best way to adjust ammonia injection and maintain the correct
pH range is with closed loop control. By configuring the pH monitor system to
control the ammonia injection, changes in control can be instantaneous and
operators can be freed from the responsibility of frequent adjustments. Obviously this approach can only be implemented when a reliable on-line analyzer
and ammonia delivery system are in place. Once this is established and the loop
has been closed, periodic checks will be necessary to ensure that the system is
working properly.
Monitor the salt content of desalted crude and the chloride content of accumulator drum water.
Continuously monitor corrosion with probes located at the inlets and outlets of
the overhead exchangers, and other areas that show signs of corrosion.
Be alert for changes in process conditions that might indicate a need for additional monitoring or a shift in the corrosion control program. For example, note
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any large change in overhead vapor line temperature or a change to a new crude
that is difficult to desalt.
Inspect overhead piping onstream and equipment during turnarounds to identify any problems or inadequacies in the corrosion control program.
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where the columns have been corroded to their minimum allowable thickness as a
result of many years service, either carbon steel or Type 405 stainless steel linings
may be applied, depending on the level of corrosion rate encountered.
However, in the newer crude units which process sour crudes at high temperatures,
significant corrosion of carbon steel is anticipated in sidecut strippers operating over
600F. For this reason, Type 405 or 410S steel cladding and internals have been
used in the hottest sidecut strippers in our newest plants.
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Carbon steel
5% chrome steel and either 12% Cases and impellers, respectively, for handling
chrome steel or CA6NM
residuum and heavier sidecuts where corrosion
is due to sulfur components
Austenitic stainless steel
Ni-resist
3170 References
Chevron Corporation
1.
2.
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3.
4.
Schmidt, P. C., and J. W. Skogsberg. Crude Unit Overhead Erosion - Corrosion Richmond Crude Unit No. 4 Data Evaluation, Chevron Research and
Technology Company Report, Materials and Equipment Engineering File
No. 75.16.56.02, January 6, 1978.
5.
Piehl, R. L. Naphthenic Acid Corrosion in Crude Distillation Units, Materials Performance, Vol. 27 No. 1 (January, 1988), pp. 37-43.
6.
7.
Shargay, C.A., Naphthenic Acid Corrosion, Chevron Research and Technology Company Report, Materials and Equipment Engineering File
No. 16.20.55.02, May 25, 1983.
8.
Crude Unit Best Practice Atmospheric Overhead Corrosion Control, originally published on Lotus Notes, also Chevron Research and Technology
Company, Materials and Equipment Engineering File No. 75.16.56.02,
June 21, 1995.
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