Customized aMDEA Process for Acid

Gas Removal

The operational experience with aMDEA gas scrubbing units shows that they contribute substantially
to both the reliability and the economy of the ammonia plant.

R. Hugo, H. Meissner, and R. Welker

BASF AG, Ludwigshafen, Germany

Introduction Process History

T
he CO2 removal system represents a major
energy consumer in an ammonia plant. An
energy-efficient gas scrubbing process is thus
sine qua non for economic production. On the other
hand, the economics of the ammonia plant also require
high on-stream times. Each extra plant shutdown due
to a failure of the CO2 removal unit causes a consider-
able loss of production and adversely affects plant
safety. For these reasons, the selection of BASF's
aMDEA process can make a substantial contribution
to both the reliability and the economy of the whole
ammonia plant.
Assuming that U.S. ammonia producers are already
well acquainted with aMDEA, this article will briefly
recapitulate the applications and process features,
which will subsequently be illustrated by a detailed
consideration of two examples of retrofitting existing
CO2 removal units (with all the inherent system con-
straints this task implies.
The development of the aMDEA process was started
in the late 1960s. The first aMDEA unit went on-
stream in 1971 with the commissioning of the No. HI
ammonia plant in Ludwigshafen, Germany. In the fol-
lowing years, eight more BASF plants were fitted with
aMDEA gas scrubbing units.
The operational experience with these aMDEA units
provided the incentive to license the process from
1982 onward. To date, the aMDEA process has been
operated successfully in a total of 66 reference plants
worldwide, with some 20 additional units currently
being under design or construction.
Applications
The aMDEA process is suitable for a wide range of
applications (Figure 1). Besides removing CO2 from
ammonia synthesis gas, aMDEA units can be used to
purify CO/H2 synthesis gas, to sweeten natural gas,

AMMONIA TECHNICAL MANUAL 330 1997

and for speciality applications such as purification of
blast furnace gases.
40% of all aMDEA reference units are to be found
in ammonia plants; more than half of these were in
turn originally operated with alternative solvents and
converted to aMDEA to solve various operating prob-
lems encountered with the former solvents.
Process Features
The aMDEA solvent systems are aqueous solutions
of the effectively nonvolatile methyldiethanolamine
plus a small amount of an activator to enhance the
CO2 absorption rate (Figure 2).
Generic MDEA reacts with water and CO2 to yield
the corresponding protonated species and bicarbonate
(Figure 3). The overall rate of conversion is very low.
The absorption can be accelerated by the fast reaction
between CO2 and the activator, a secondary amine,
which together form a carbamate. The carbamate in
turn reacts with the bulk solvent (aqueous MDEA)
transferring its CO2 and thereby being regenerated for
further reaction. The activator therefore behaves in a
similar manner to a homogeneous liquid catalyst with
no net consumption, but rather several reaction-regen-
eration cycles along the length of the absorber.
The high loading capacity of MDEA results in low
solvent circulation rates, while the activator keeps the
absorber height to a minimum. The solvent regenera-
tion can be carried out to a large extent simply by
flashing the aMDEA solution.
An extra degree of flexibility is achieved by varying
the activator concentration (Figure 4). This has the
effect of tuning solvent behavior to either a more
"chemical" or a more "physical" character. The highly
activated MDEA 06 has more of a chemical solvent
nature, that is, good absorption efficiency but energy
intensive regeneration, while the weakly activated
MDEA 01 has only a moderate absorption efficiency
but benefits from an energy efficient regeneration,
similar to that for a physical solvent.
Typical application criteria for CO2 removal from
ammonia synthesis gas are:
• aMDEA types 02 thru 04 in a standard two-stage
unit, characterized by low energy consumption values,
high gas purities, and good recovery rates (Figure 5);
AMMONIA TECHNICAL MANUAL
• aMDEA types 04 thru 06 in a standard single-stage
unit, characterized by reduced investment costs and
very low CO2 slippage in the treated gas (Figure 6).
The number of aMDEA solvent systems combined
with a variety of appropriate process configurations
ensure a design tailor-made for a given application, be
it a revamp or a new plant.
Retrofit of Acid Gas Removal Units
For the "grassroots" design of a new plant, the sol-
vent, the configuration, and the process parameters
can be customized to meet all production and site
requirements. For a revamp, however, the design
needs considerable process flexibility to conform to a
given application. Many additional constraints result
from the equipment already installed and the integra-
tion of the unit in the ammonia plant. The following
examples illustrate such situations.
The first example involves typical conditions for the
U.S. reference plants, all of which entailed conver-
sions of ammonia synthesis gas scrubbing units to
aMDEA (Figure 7). The second example describes the
revamp of a hot potassium plant in Australia.
Conversion from an amine-based solvent
The U.S. references are all ammonia plants with a
capacity in the range 650-1,500 mtpd, and all have a
background similar to that of the unit portrayed in the
following example. The gas scrubbing unit comprises
a single-stage absorption and stripper regeneration
(see Figure 6) and was originally operated with
monoethanolamine (MEA).
This unit has been converted to another amine based
system in the context of a capacity increase. The alter-
native of achieving a higher plant capacity by an
increase of the MEA concentration was ruled out by
the operational experience regarding the corrosivity of
the MEA solution, especially at higher concentration.
Understandably, the corrosivity of the solution was
investigated extensively. Following the swap, solvent
analyses showed no untoward heavy metal content in
the solution for the first year. Thereafter, some weight
loss was observed on the corrosion coupons and sub-
sequently a steep increase in the concentration of
331 1997
 Figure 1. Application of BASF's aMDEA-process. Figure 2. Activated MDEA solvent system.

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Figure 3. Absorption mechanism. Figure 4. CO2-loadmg capacity of various solvents.

AMMONIA TECHNICAL MANUAL 332 1997

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Figure 5. Two-stage absorption. Figure 6. Single-stage absorption.

Figure 7. Plant locations. Figure 8. Damaged tubes from the four

exchangers.

AMMONIA TECHNICAL MANUAL 333 1997

heavy metals (Fe, Cr, Ni) in the solution took place. tubes from the four exchangers.
Corrosion problems occurred especially in the solvent The shell of the lean solution cooler (solvent on
heat exchangers (2 parallel stacks, each of 2 individual shellside) also exhibited wear-and-tear, probably as a
exchangers) and in the regenerator (duplicate parallel result of erosive corrosion.
tray columns) along with several additional shutdowns Special attention must be paid to the feed device of
and the need to replace corroded equipment. The
hopes placed in this second solvent thus proved to be Table 1. Heavy Metal Content of the aMDEA
unfounded, as the unit still suffered from leaks due to Solution
corrosion.
At this point, a straight solution swap to aMDEA Months of Cr Ni Fe
was carried out without any plant modifications. In a Operation (wppm) (wppm) (wppm)
rapid turnaround, the previous solvent was drained off,
the unit cleaned, filled with aMDEA solution and 7 7 1 7
restarted. 11 1 1 5
13 1 1 4
Equipment inspection after draining off the previ- 16 2 1 7
ous solvent 20 3 2 6
23 2 1 5
No Corrosion was detected in the absorber column. 1 4
26 5
The stripper columns showed corrosion in the bot-
29 4 6 6
tom sections and between the trays. The corrosion was
of a local nature, being characterized by cavities of 2 33 5 8 4
in. (5 cm) diameter and up to 2/5 in. (1 cm) depth from
a height of approximately 6.5 ft (2 m) up to the loca-
tion of the packing support grid. The material around the regenerator when converting a chemical solvent to
the cavities was friable and could easily be removed aMDEA: about 30-50% of the CO2 is released from
mechnically. The material within the manhole showed the rich solution by depressurization. The degassing
similar corrosion effects. therefore starts just downstream the pressure relief
The stripper reboiler heads were damaged with the valve and continues in the upper section of the regen-
pitting corrosion characteristic of hot CO2/water vapor erator. In a tray column flashing takes place on the top
attack. tray. The flashing solution, however, shall not enter
The four solvent heat exchangers are fitted with the downcomer, as degassing in the downcomer can
stainless (SS) tubing and carbon steel (CS) shells. result in flooding of the column. In case the regenera-
Although the expansion valve is located downstream tor is fitted with packing, the existing distributor must
the solvent heat exchangers, degassing of CO2 of the be adapted for the operation with a flashing feed. At
rich solution most probably occurs, which results in a any rate, the disengagement zone above the feed
two-phase flow through the exchangers, giving rise to device must be sufficiently high hi order to avoid solu-
severe corrosive attack: In the exchanger heads (pre- tion entrainment.
dominantly at the hot end) pitting corrosion was
observed over the entire CS material (about 2 mm Precleaning and repair work
depth) as well as at the welds (4 mm depth). Even
though the tubes were of SS, about 10% leaked. The system was cleaned section by section: first
Corrosion was confined to within the tubes, as the opening manholes and bottom drains of columns and
outer surface still appeared to be in good shape. The tanks, then removing orifice meters in the liquid lines
CS elements used to support the tube bundles were after closing off the taps hi impulse pressure line con-
extensively corroded. Figure 8 depicts the damaged nections beforehand and finally flushing the equip-

AMMONIA TECHNICAL MANUAL 334 1997

 Figure 9. Corrosion rates in bottom of stripper. Figure 10. Revamp of hot-pot unit in Australia.

Non-corrosive solvent
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^ f^ f^^ff ' " f ••'">•• * S S-, SS - ff f f * * / ' J f -,-,* , , - , * ,

;-, * Signlficantiy lower thermal energy consumption

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>J' No environmental, problems'
•'' ï Minimum- analytical requirements-
,'-/,; Easy to operate/'very '*forglvlog*;;and; robust process'

11. aMDEA compared to hot potassium carbonate systems.

AMMONIA TECHNICAL MANUAL 335 1997

ment with water using firehoses and/or water jets. The
heat exchanger tube bundles were removed and
cleaned with a high pressure water jet. Particularly the
tubing in the solvent heat exchangers showed a firm
deposit layer inside the tubes, which could neverthe-
less be removed with a caustic solution jet. The outer
surface of these tubes was covered with a grayish-
brown layer (most probably FeCO3) after cleaning,
which could also be removed easily.
The corroded equipment surfaces were washed off
with a water jet. Corrosion cavities were then hollow-
grinded, polished and repaired with a corrosion protec-
tion layer (0.6-1 mm thickness) applied by a thermal
metal spraying procedure. The bottom section of the
stripper columns was covered with metal dust from the
spraying procedure, and the trays and the column base
had to be cleaned with a vacuum cleaner.
Cleaning procedure prior to startup
The two stripper columns were flooded with con-
densate and then drained. This procedure was repeated
once more with samples being taken to check for the
absence of residual suspended particles in filtration
tests.
Afterwards, the whole unit was filled with conden-
sate, heated up to 176-194°F (80-90°C) and circulated
for 4 h, with about 10% of the flow rate passing
through the mechanical filter. The condensate analysis
after 4 h circulation showed no foam activity or sus-
pended particles, and the sample had a yellowish-
brown coloration. The condensate circulation proce-
dure was repeated, with the sample showing no decol-
oration as a result.
The cleaning efforts can be reduced or enhanced
depending on the very situation and the history of each
plant. In this case, for instance, the system was not
flushed by circulating caustic solution or dilute
MDEA solution as usually recommended, especially
for the removal of grease or other residues such as cor-
rosion inhibitors, rust, and so on. The caustic flushing
should, however, be employed when considerable con-
struction work has been carried out, if new equipment
has been installed or if the entire plant is new.
Startup
AMMONIA TECHNICAL MANUAL
The system was checked for leakages and put under
nitrogen pressure. The aMDEA premix was introduced
from tank containers into the system and diluted with
water down to 45wt.% amine concentration. The sol-
vent loop was closed, defoamer was added, and the
circulating solvent was heated up to the design condi-
tions. The gas throughput was set to 75% of the design
capacity. Within 3 days, a capacity of 108% could be
achieved and the conditions (energy, solvent, flow
rate) had been optimized to meet the design CO2 slip
of 20 vppm.
Operating experience after the swap
The corrosion attack associated with the previous
solvent is clearly indicated by a material loss from the
test coupons in the mm per year range (Figure 9).
After the revamp to aMDEA, the corrosion was com-
pletely eliminated, without needing to add any corro-
sion inhibitor. In contrast to the previous solution, the
heavy metal content of the aMDEA solution (as tabu-
lated in Table 1) was kept virtually constant in the low
ppm range.
Other amine-based systems (such as MEA, DEA,
DIPA) have also been successfully converted to
aMDEA with considerable energy savings achieved
and a complete eradication of earlier corrosion prob-
lems. The demands on the flexibility of the solvent,
however, are considerably higher if the solvent being
replaced is of a completely different nature to an
amine solution, as in the following example.
Conversion of a hot potassium carbonate unit
The second example deals with the very first revamp
of a hot-potassium carbonate unit to aMDEA. The 720
mtpd ammonia plant in Australia comprised a two-
stage hot-pot gas scrubbing unit. Toxic arsenic salts
were used both for activation and corrosion inhibition.
In recent years, sections of the pipework and packed
beds had to be replaced owing to the corrosivity of
the hot-pot solution.
The main problems, however, were escalating costs
for disposal of the arsenic-containing purge stream and
the presence of arsenic in the plant wastewater.
The process configuration and the operating condi-
336 1997
lions of this Australian hot-pot unit (Figure 10) are
significantly different from a standard two-stage
aMDEA unit (see Figure 5):
• No lean/semilean solvent heat exchanger.
• Ratio semilean to lean solvent flow rate 4.5 vs. 6-7
for aMDEA.
• Lean solvent temperature of 169°F (76°C) vs.
122°F (50°C) for aMDEA.
• Semilean solvent temperature of 234°F (112°C) vs.
167-185°F (75-85°C) for aMDEA.
Table 2. Three Consecutive Flushing Steps Using
NaOH Solution
NaOH Circulation Max. Arsenic
(wt.%) 00 (wppm)
4.0 8 1,900
3.9 8 160
1.7 6 60
• Low pressure flash fitted with packing of about 3
times the height as for aMDEA.
• Density of hot-pot solution approximately 25%
higher compared to aMDEA.
Generally, the main challenge for the solvent con-
version of hot-pot units arises from the considerably
lower temperature level in the absorber and the lower
aMDEA density. Both factors typically lead to bottle-
necks due to a lack of cooling capacity (most units do
not even have a semilean solution cooler!) and inade-
quate capacity in the solvent pumps.
Process modifications
For the above reasons, a straight solution swap (as
described in the section on conversion from an amine-
based solvent) is not usually feasible. The following
modifications had to be carried out for this Australian
revamp assignment.
• At full capacity, the suction pressure of the lean
solution pump (when operated with aMDEA) would
have fallen below the required limit. To provide suffi-
cient head for the less dense aMDEA, a lean/rich sol-
AMMONIA TECHNICAL MANUAL
vent heat exchanger was installed to cool the lean
solution from the stripper bottom and the lean solution
pump was operated at higher speeds. A peculiarity of
the solvent heat exchanger (in contrast to the
lean/semilean solvent heat exchanger of the standard
design (see Figure 5)) is the shellside flow of CO2-
loaded rich solution and the tubeside flow of the lean
solution. This arrangement was chosen in order to take
into account the high ratio of rich to lean solution in
the operation of the existing unit. CO2 is thus released
by heating up the rich solution in the exchanger. A
lean solution air cooler instead of a solvent heat
exchanger was not a practical alternative due to the
higher space requirements, and an additional water
cooler was ruled out by the increased water consumption.
• The duty of the existing lean solution cooler was
increased by providing cooling water at a lower tem-
perature. The lean solution temperature could be
reduced from 169°F (76°C) to 158°F (70°C) in this
way, thus giving rise to a higher solution loading
capacity and a reduced solvent flow rate. By this
means, the aMDEA design was rendered compatible
with the capacity limits of the existing pumps.
• The hot-pot unit was operated at a process gas tem-
perature of 433°F (223°C). As such conditions are
beyond the operational experience of aMDEA refer-
ence units, it was decided to install a process gas cool-
er upstream of the regenerator gas reboiler to reduce
the absorber inlet gas temperature down to 329°F (165
°C). A gas inlet temperature of 329°F is still adequate
to operate the regenerator properly since the energy
consumption is much less for aMDEA. The new heat
exchanger is part of a reformer feedstock saturator
scheme, thus providing energy recovery from the feed
gas.
9
The lean absorber section was fitted with
polypropylene packing, which was severely deformed.
The two PP packed beds have now been replaced by 1
in. S.S. TP304 rings.
• Parts of the piping showed corrosion and were
replaced by SS TP304 lines.
« About 80% of the released CO2 was previously
vented to the atmosphere at 194°F (90°C).
Only 20% of the CO2 was cooled down to 113°F (45
°C) condensed and processed up to foodgrade quality.
An additional CO2 cooler, reflux drum, and reflux
337 1997
 Table 3. Comparison of Operating Data for the Hot-Pot Solution
Hot-Pot Solution aMDEA Solution

Feed gas 185°F (85°C) 185°F

429 psia (29.6 bara) 429 psia
18 vol.% CO2 18 vol.% CO2
CO2 slip <500 vppm <500 vppm
Lean solution 169°F (76°C) 158°F(70°C)
Semilean solution 234°F(112°C) 180°F (82°C)
Absorber bottom 226°F (108°C) 203°F (95°C)
Process gas reboiler in operation in operation
Steam reboiler in operation not in use
Specific energy consumption 49.9 mbtu/lb mol CO2 32.7 mbtu/lb mol CO2

pump were installed parallel to the existing reflux cir-
cuit in order to provide a moderate temperature of the
CO2 off-gas stream, thus limiting the vapor phase sol-
vent losses.
Cleaning of the Unit
The unit had been operated with a hot-pot solution
since 1969 using arsenic salts as corrosion inhibitor
and activator. It was therefore to be expected that con-
siderable amounts of precipitated corrosion products
(deposit of iron/arsenic complex) were deposited on
equipment surfaces. There were some concerns
regarding the fact that aMDEA is known to dissolve
such deposits quite well, which might have increased
foaming susceptibility and carryover of the solution
from the regenerator into the condensate reboiler.
The cleaning procedure was carried out as follows:
« Three consecutive flushing steps using NaOH
solution at 194°F (90°C), each of which was broken
off after the arsenic content had attained its maximum
are shown in Table 2.
• Two consecutive water flushing steps were at
194°F (90°C); the water analysis after the second
flushing step gave 60 wppm iron, 7 wppm arsenic, 80
wppm NaOH and 100 wppm solids and the sample
exhibited a dark brownish color. The solids were iden-
tified as very fine rust particles (probably iron/arsenic
complex) in the size range 5-50 urn; the foam test with
aMDEA indicated a significant foaming tendency.
• A further water flushing step was not carried out in
order to limit the amount of arsenic contaminated
flushing water. It was decided to allow for the higher
foaming tendency by running the mechanical filter (5-
10 u,m cartridges) at its maximum throughput from the
very beginning of the solvent circulation and employ-
ing an appropriate defoamer dosage rate.
Startup
The unit was filled with aMDEA premix and the
water content and column levels adjusted by adding
condensate.
The solvent circulation was commenced at about
50% of the design flow rate. After 12 h of circulation,
the solution had a reddish-brown color and a foam test
indicated formation of very stable foam (collapse time
more than 5 min). After filtering the aMDEA sample,
the color turned light yellow and the foam activity was
reduced to the normal values.
An extra dose of defoamer was introduced into the
solution loop and the circulation rate increased to 95%
of the design figure: the column levels became unsta-
ble and hence a further shot of defoamer was added.

AMMONIA TECHNICAL MANUAL 338 1997

The column levels remained constant and the next
foam test showed no significant foaming tendency.
The solution circuit was heated up to the design val-
ues with the regenerator steam. The CO2 cooler and
reflux pumps were put into operation. The semilean
and lean solvent temperatures to the absorber were
adjusted at a later stage when the solvent coolers were
started up.
Process gas was fed through the plant at 50% capac-
ity. Within 12 h, the plant throughput was increased to
80% of the design figure. Process conditions were
then optimized at full capacity.
Although the process conditions of a hot-pot system
differ significantly from aMDEA units, the aMDEA
design for this unit showed a good compatibility with
the existing equipment. A comparison of the operating
data for the hot-pot solution and the aMDEA design
for 100% capacity is tabulated in Table 3.
A summary of the benefits from the 1994 solvent
conversion is given in Figure 11:
• The aMDEA solvent does not require the addition
of any corrosion inhibitor. Hence, the costly disposal
of toxic arsenic-material (inherent for the hot-pot sys-
tem) is completely avoided. Even the time-consuming
passivation of the equipment prior to a startup of the
hot-pot system can be omitted, thus keeping the turn-
around periods to a minimum.
• Although the process conditions are not cus-
tomized for the aMDEA solvent system, the energy
saving is still 35% compared with the hot-pot opera-
tion.
• The operator workload is lightened as the intense
supervision required for operation of the hot-pot unit
is no longer necessary. Precipitation does not occur
with aMDEA; thus, heat tracing is not required. The
revamped unit is operated with virtually no liquid
purge stream, as there is no need to separate decompo-
sition products or to purge the solution thereof. The
plant monitoring has been reduced to a minimum, with
only a few simple analyses remaining to be carried
out.
Operational Experience
The flexibility of the aMDEA process also offers
attractive operational features.
AMMONIA TECHNICAL MANUAL
BASF operates two ammonia plants in
Ludwigshafen, Germany: Both plants No. HI and No.
IV, a 1,350 mtpd unit, which have come on-stream in
1971 and 1982, respectively, are equipped with low-
energy two-stage aMDEA systems (see Figure 5).
Following a capacity increase some years ago, the
gas scrubbing unit of the No. IV plant was being oper-
ated at the limits of the certain existing equipment
items such as solution pumps and columns. A second
plant expansion of 6% was recently carried out with-
out any equipment changes or capital costs being
involved.
The activator content in the solution was increased
slightly, thus leading to a higher absorber efficiency by
shifting to more chemical solvent characteristics. As
the activator could be added during operation, no shut-
down was necessary.
Conclusion
This article deals with a specific range of aMDEA
applications, namely the conversion of solvents in
existing ammonia plant gas scrubbing units.
Units which are designed to be operated with amine
based solvents can most often be converted to aMDEA
in a straight solution swap: the old solvent is drained
off, the system is cleaned, filled with aMDEA premix,
made up with condensate, started up (faute de mieux
with the old conditions), and optimized.
The conversion of units designed for solvents with a
totally different nature to amine solutions normally
requires some equipment changes, however. Hot
potassium revamps, for instance, are characterized by
a lack of adequate cooling and pump capacities.
Furthermore, the heat integration of the gas scrub-
bing unit within the whole ammonia complex can
exert constraints determining the operating conditions
at certain locations in the unit, such as boiler feedwa-
ter heaters (T, dT, heat duties, and so on). This can
turn out to be a bottleneck, for instance, due to differ-
ent physical and thermal properties of the solvents.
The flexibility of the aMDEA process takes account of
such constraints by allowing one to change the funda-
mental nature of the solvent. Even if such a revamped
unit cannot be operated at the optimum conditions
when compared to new, grassroots aMDEA units,
339 1997
advantages still accrue, that is, no corrosion, energy
efficiency, and no purge stream disposal.
The straight solution swap in the U.S., the revamp of
the hot-pot unit in Australia, and the capacity increase
of BASF's ammonia plant in Ludwigshafen provide
AMMONIA TECHNICAL MANUAL
three illuminating examples of the economic efficiency
and reliability of the aMDEA process, which is further
characterized by the cardinal virtues of being environ-
mentally friendly, easy-to-operate, and very forgiving,
340 1997