Optimizing heat transfer

uid performance
How to avoid costly consequences
Conrad Gamble, P.E.
Matthias Schopf
Contents
Introduction ............................................................................ 02
Selection of the proper uid for the application .... 02
Measuring the six key parameters of in-service
uid quality ...................................................................... 04
Additional considerations ................................................. 05
In-use monitoring and actions ........................................ 06
Summary .................................................................................. 10
About the authors ................................................................ 11
References ............................................................................... 11
Introduction
Even a perfectly designed and installed heat
transfer uid system is vulnerable to
operational stress factors which can
deteriorate its performance and can reduce
uid and system component life times. Heat
transfer uids are an essential component of
the operation of many high-temperature
processes. When the heat transfer uid isnt
performing up to expectations, there can be
detrimental impacts to product quality,
production rates, heat transfer uid, and
equipment life and it can consume resources
in troubleshooting. With the following helpful
concepts, a knowledgeable engineer can
effectively anticipate and manage these
factors and avoid costly consequences.
Selection of the proper uid
for the application
Securing the best and most enduring performance from
your uid actually begins with features beyond the uid
itself. The users of a heat transfer uid should source
their uid from a reliable, reputable, and responsible
supplier. Pay attention to feedback heard from
distributors, independent specialists, and other users who
have had prior experience with the various suppliers, so
that you can benet from the advantages provided by
manufacturers who have a well-established track record,
who have well-networked supply and distribution chains,
and where experienced customer support specialists
answer the phones live when you need them. You can
also use this feedback to avoid some of the pitfalls that
might be present with lower-tier suppliers and uids.
Keep in mind that some suppliers may only be
distributors or remarketers who have very limited
product and application knowledge. It is always best to
buy from the uid manufacturer having the experts on
staff who can answer just about anything related to the
safe and effective use of the uid and its chemistry, or
from a distributor having well-trained sales personnel
and a strong alliance with the manufacturer.
2
Engineers will need accurate technical data and physical
properties to help support design and troubleshooting
efforts. Today, this information is almost always readily
available for downloading from web sites, but the
technical data should be reviewed as part of the uid
selection process to ensure it provides the needed level
of detail. Engineers need quality data, and not just
smoothed curves on low-resolution graphs. For safety
and environmental evaluations and response, make sure
current and complete Safety Data Sheets are also
available from the supplier.
Also, the plant engineers will require the suppliers
analytical support to run the proper tests on the in-
service uid samples, and have the expertise to fully
interpret the test results for providing guidance on when
uid quality adjustments might be necessary, extending
the good performance life of the uid to its maximum.
Experienced technical service engineers from the uid
supplier should be able to recognize the early stages of
developing problems and counsel the plant engineer on
the potential causes so they can be corrected at their
earliest and before costly problems develop.
What are those potential uid-related problems that
users might experience? Problems can develop which
will be associated with changes in uid chemistry and its
physical properties when the uid quality deteriorates
(ages) from use or contamination. These can include
increased corrosion risk, fouling potential, solids/sludge
formation, and pumping difculties.
To best resist the effects of uid aging and potential
system impacts, using a high quality uid is the
appropriate starting point. The following attributes
should be considered:
Demonstrated performanceSince the heat transfer
uid is the life blood of the high-temperature process,
it pays to buy a quality uid and chemistry to meet the
requirements. Consult the uid supplier and others on
the performance records of prospective uids. Weigh
this feedback against the needs of the application, giving
due consideration to operating temperature, on-stream
time, plant location (for cold start-up factors), possible
future higher-temperature requirements, and if other
heat transfer uid systems are at the same plant site, for
common uid inventory stocking.
Clearly dened sales specicationsOne means of
quality assurance for the end user is the product sales
specications provided by the manufacturer. If needed,
the manufacturer should also be capable of issuing
certicates of analysis or conformance that the
delivered uids meet those specications each and
every time.
ISO-9001 certied processesCustomers are also
protected by manufacturers who have invested in
strictly controlled processes certied by independent
auditors. If the supplier can provide such certication,
such as ISO-9001 conformance, the end user can have
added condence in product consistency.
Reliably advertised temperature ratingsThe
method of establishing maximum bulk temperature
ratings of heat transfer uids is not mandated by
industry standards and is left up to the uid
manufacturer or marketer to assign. There are
established test methods for measuring thermal
stability of organic heat transfer uids,
i,ii
but they stop
short of prescribing the translation of those results into
the published temperature ratings. Consult the uid
supplier about the expected life of the uid when
operated at the maximum temperature rating or at the
expected operating temperature for the process. For
example, some suppliers may rate the maximum bulk
temperature to provide a two-to-three-year life
expectancy, where other suppliers may choose to rate
for a longer life which could result in a somewhat lower
published maximum temperature rating. Keep in mind
too, that how the process is operated can inuence the
actual uid life experienced. For example, frequent
power interruptions can create very thermally stressful
conditions for heat transfer uids that can greatly
shorten uid life even if the normal maximum
operating temperature is well within the published
maximum bulk temperature limit. Lastly, it should be
factored into the uid selection decision that if a
maximum bulk temperature rating is exceeded by
roughly 10C (18F), the thermal stress is also roughly
doubled. This can be expected to signicantly reduce
uid life expectancy. Conversely, reducing the operating
temperature by the same amount from the maximum
bulk temperature rating can be expected to reduce
thermal stress by roughly half, thereby signicantly
increasing the uids life expectancy.
iii
3
Physical propertiesThe physical properties (liquid
viscosity, thermal conductivity, heat capacity, and
density) will be evaluated when determining heat
transfer coefcients in support of heat exchange area
required, however also consider the vapor pressure of
the uid. Lower system pressures will promote efcient
low-boiling degradation products venting and will
inherently tend to be less of a leakage problem.
A uid with suitable viscosity at the lowest expected
temperature for winter start-up can avoid investment
into heat tracing and vessel heating, as well as
oversized pump motors.
iv
Fluids having freezing points
above the lowest temperature possible will require
incorporation of freeze protection into the system
design, including the protection of instrumentation
sensing lines, and overpressure protection devices.
Measuring the six key parameters
of in-service uid quality
The following are considered the most important measures
that can indicate developing problems, enabling potential
corrective actions to protect uid performance/life.
1. Viscosity can be readily measured in a uids lab,
typically by ASTM-445,
v
or similar technique. In the
ASTM D-445 method, a uid sample is held at a
precisely controlled temperature while the time for a
known volume of the uid to pass through a calibrated
tube is measured. From the elapsed time, the viscosity
is calculated (Figure 1).
2. Moisture content is typically analyzed by the Karl
Fischer titration technique.
vi
Moisture content should
be kept quite low when operating at high temperatures
to avoid issues related to its ashing into water vapor.
Inability to maintain low moisture content is an
indicator of either an aqueous leak into the system,
or perhaps the addition of wet make up uid.
3. The ash point of a high-temperature uid is
commonly measured by the Cleveland Open Cup
(COC) method, ASTM D-92.
vii
A closed cup technique
is also useful in classifying uids and is run per ASTM
D-93.
viii
The ash point is the lowest temperature of
the uid under the test conditions where ignition of
the vapors above the liquid can occur, yet evaporation
rate is too low to sustain combustion. Flash points
are important in electrical classication and hazard
analysis. (Figure 1)
4
4. Acidity of uids is commonly measured by ASTM
D-664,
ix
which is a potentiometric titration. Fluid
oxidation results in accumulations of carboxylic acids
which lower the apparent pH or raise the total acid
number (TAN). Typically, unused organic heat transfer
uids will have a near zero acid number. (Figure 1)
5. Insoluble solids content is essentially a measure of
the concentration of solids in the uid at room
temperature. Of particular importance are the organic
solids which result from exceeding their solubility
limit in the uid. Other solids can include carbon,
small portions of gasket materials and metal shavings,
and some rust.
6. Composition/degradationGas chromatography
allows the quantication of compounds which
have boiling points lower than the initial boiling point
(low boilers [LBs]) and higher than the nal boiling
point (high boilers [HBs]) of the unstressed uid. This
analysis provides a measure of the degree of uid
degradation experienced and can provide an indicator
of organic contamination. Gas chromatography
typically cannot directly provide a measure of
inorganic contamination of organic uids.
Additional considerations
The proper selection of heat transfer uid for the
process should also consider the potential of intermixing
of the process stream(s) with the heat transfer uid. If
this occurs, would chemical interaction be expected?
Can the two be effectively separated? Will the integrity
of system components be compromised due to chemical
incompatibilities?
In general, when a uid is chosen from a very reputable
and established supplier which has the requisite quality
assurance systems built-in to its supply chain, has the
performance properties and thermal stability well-matched
to the application requirements, and where the uid
quality is supported by periodic expert analysis, the new
process has the pieces in place for an optimally performing
heat transfer uid. The remaining task is to properly
monitor and maintain these advantages over time.
5
Figure 1Typical instruments for measurement of density and viscosity,
ash point, and total acid number (left to right).
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In-use monitoring and actions
In the preceding sections, we have indicated that heat
transfer uids properties may change, such that actions
would be recommended to either extend the service life
of the uid or prevent occurrence of deteriorating system
performance.
x
For each uid property analyzed, the
supplier of the heat transfer uid may have established
specic warning or action limits. Such uid property
limits, provided together with recommendations in an
evaluation report, are a composite of the experience in
the analyses of used uid samples and knowledge about
heat transfer uid degradation mechanisms. The actual
thresholds for operational problems can vary depending
on specic system design factors including inert gas or
system pressure, pump NSPHA and NPSHR, pressure
drops, etc. In general, when the test results all fall into a
normal range, the uid is probably in good condition. If
one or more of the tests fall into the warning area, the
system operator may consider taking appropriate action
such as venting, ltration, etc. When the results fall in the
action area, taking action to return the uid to a more
normal condition either by appropriate uid treatment or
complete drain and rell is more of a necessity.
Understanding that establishing such limits is a composite
of experience and that specic system requirements may
call for different limits, its quite understandable that
such limits should not be considered to be rigid. This
meanstaking as an example a low-boiler upper limit of
5%that there is no guarantee that systems operating
at a low-boiler concentration, e.g., 4.8%, will not
experience operational problems such as increased vapor
pressure, pump cavitation, or signicant ash point drop,
but a system operating at a level of 5.2% of low boilers
will suddenly suffer from these consequences. Also, it is
important to understand that uid properties and their
limits should not be evaluated independently of each
other. For example, a system exhibiting a high-boiler
content close to or even slightly above the action limit
but having the viscosity and insoluble solids content in
the normal ranges may not require immediate actions.
Nevertheless, the key properties and corrective actions
for signicant deviations of each uid property measured
individually are discussed in the following. A summary is
provided in Table 1, page 10.
1. Viscosity
The uids viscosity is a measure of its resistance to ow.
Fluids of greater viscosity will require higher-pumping
horsepower requirements and will adversely affect the
degree of turbulence at heat exchange surfaces which
can lower heat transfer coefcients. Not only can
elevated viscosity reduce heat transfer performance at
high temperatures, it can also affect the ability to pump
the uid during cold weather start-up conditions.
Viscosity is related to the molecular weight of uid
components. Generally, lower molecular weight
components decrease viscosity and higher molecular
weight components increase viscosity of the heat
transfer uid. Contamination from leaked process
streams, incorrect material added to the heat transfer
uid system, and solvents from system cleaning, as well
as thermal stressing and oxidation, may be the source of
materials that increase or decrease viscosity. Regardless
of any action taken, the causes of viscosity changes
should be determined. The typical corrective action to
6
address too low a viscosity would be the removal of low-
boiling components by circulating the heated uid
through the expansion tank with inert gas purge of the
vapor space while venting to a safe location (Figure 2).
Condensation and collection for proper disposal of the
removed low-boiling organics is recommended unless
vented to a properly designed are. Correcting for
high viscosity requires either aged uid removal and
replacement or dilution with unused heat transfer uid.
2. Moisture
When operating at very high temperatures, excess
moisture content can prevent the ability to circulate the
heat transfer uid due to its ashing into vapor at the
circulation pump intake, creating cavitation. Extended
operation with cavitation can lead to excessive heat
transfer uid degradation in heater coils due to lower
mass ow rates delivered from the pump. Also corrosion
may be induced by elevated concentrations of system
moisture. In cooling systems, a high moisture content of
the uid will increase the risk of formation of ice crystals
on chiller surfaces. This can decrease the efciency of
heat transfer and deteriorate the overall system
performance. On new system start-ups, it is important to
remove residual moisture from the system (from
hydrostatic testing) to enable the uid to heat fully to
the desired operating temperature. For systems in
operation, increasing moisture content may be caused by
in-leakage of water from aqueous process steams or from
steam systems, or by moisture intake via an expansion
tank open to atmosphere. Excess moisture can typically
be vented from the expansion tank using the low-boiler
venting method (see 1. Viscosity, p. 6). To achieve low
ppm moisture levels required for the cooling operation,
molecular sieves can be placed in side stream operation.
3. Flash point
While many heat transfer uids have relatively high ash
points, they often are not classied as re resistant.
However, heat transfer uid systems are usually closed
systems. Therefore, a release of uid should only occur in
case of accidents or malfunctions and it is typically safe
to operate such well-designed and maintained systems
and uids even at temperatures well above the uids
ash point. Flash point is a property to be considered in
the hazard evaluation of operating systems with
combustible uids. A signicantly depressed ash point
of the in-service heat transfer uid may not only increase
the re hazard in case of leakages and the presence of an
effective ignition source, it may also affect the area
electrical classication of the system in extreme cases.
Typically, routine venting of low-boiling thermal
degradation products from the expansion tank to a safe
location will maintain the uids open-cup ash point to
within 25C (45F) of the ash point of unused uid.
Relief valve
Pump
A
B C D
E
F
HLA
LLA
Fill lineoperating
Fill lineinitial (low point)
Low-pressure
regulator
Catch
pot
Vent to
safe area
Outlet
regulator
HLA = High level alarm
LLA = Low level alarm
Inert
gas
Approx. 1/3
full line size
Figure 2Features of a common expansion tank design.
7
4. Acidity
High acid numbers could indicate severe uid oxidation,
which is most often a result of hot uid exposure to air in
the expansion tank. But they may also indicate possible
contamination from improper material added to the
system inadvertently or uid leaked from the process side
of heat exchangers. If the acidity becomes excessive, the
system components could corrode and fail. Oxidation and
corrosion products can form sludge and deposits that can
also decrease heat transfer rates by fouling. A condition of
this nature is typically best corrected by removing the
material and replacing it with new uid, with serious
consideration given to a system ush to remove residual
acidity. If the high acidity was caused by oxidation,
inerting the vapor space in the expansion tank should
certainly be considered. System inerting has proven to be
a highly effective means of protecting against unwanted
increases in uid acidity and oxidative degradation.
5. Insoluble solids
The presence of solvent (typically acetone or pentane)
insoluble solids generally indicates contamination from
dirt, corrosion products, or severe oxidative or thermal
stressing. This condition may cause fouling of heat
transfer surfaces which would deteriorate heat transfer
performance. Also, plugging of small diameter lines or
narrow heat transfer passages could occur. Finally, large
amounts of insoluble solids may contribute to wear and
plugging of mechanical seals and valves resulting in
equipment failure, operational problems, and increased
maintenance requirements. If these problems occur, side
stream ltration can usually provide ongoing protection
against solids-related deposits and their potential
consequences. If solids contamination is extremely high,
uid may need to be removed for external ltration and
the system may need to be cleaned. Specialized ushing
uids, designed by heat transfer uid suppliers, can be
effective in removing fouling deposits from most
synthetic and mineral oil uid systems. Modest solids
content may require ltering with successively ner
rated lter element sizes to get the situation under
control. A suggested lter rating generally is 10 to 25
micron for ongoing uid maintenance.
Inert gas blanketing
An effective method of minimizing uid
oxidation is to blanket the expansion tank with
an inert gas such as nitrogen, carbon dioxide, or
natural gas. The purpose of inert gas blanketing
is to maintain a nonreactive atmosphere in the
vapor space of the expansion tank, preventing
the entrance of air and moisture which can
adversely affect uid life. An uninterrupted
supply of inert gas, usually nitrogen, controlled
by pressure regulators for both inlet and outlet
ow is necessary to obtain this protection.
Pressures used should be kept as low as
possible inside the expansion tank to minimize
inert gas usage. Maintaining a positive pressure
slightly over atmospheric barometric pressure
is all that is necessary to prevent air and
moisture from entering the tank. A manual
vent valve also should be installed to facilitate
purging of the expansion tanks vapor space
if it becomes necessary.
8
6. Thermal degradationlow boilers and high boilers
Thermal cracking of the heat transfer uid will result in
components which are lower in molecular weight and
commonly are known as low boilers. High boilers also
can be generated when some compounds recombine
to produce higher molecular weight materials. Both
low- and high-boiling degradation products can create
an unfavorable environment for efcient heat transfer
system operation.
a. Low boilers
Low-boiling components can affect system operation in
several ways. First, when present in signicant quantities,
low boilers can lead to pump cavitation. Severe cases
may cause damage to pump seals and, if allowed to
continue uncorrected, can damage impellers. Second,
when low boilers are present in excessive concentrations,
the heat transfer uid ashpoint and viscosity may be
lowered. Third, the increased uid vapor pressure
resulting from the presence of low-boiling components
can cause premature and unexpected pressure relief and
venting. Finally, excessively rapid formation of low boilers
will result in unacceptably high uid make up costs as
the low boilers removed from the system are replaced
with fresh uid. Removal of low boilers is typically
accomplished by venting from the expansion tank to a
safe location (Figure 2).
b. High boilers
The presence of high boilers can increase heat transfer
uid viscosity, which will affect the uids pumpability at
low temperatures and the systems heat transfer
efciency. Unlike low boilers, high-boiling compounds
cannot be removed from the system easily once they are
formed. Hence, high boilers continue to accumulate until
the maximum recommended concentrations are reached,
thereby signaling the end of the recommended uid life.
If high-boiler concentrations are allowed to accumulate
beyond that point, sludge and tar deposits can form as
the solubility limits for the higher molecular weight
compounds are exceeded. Added costs of operation as a
result of these sludge deposits include downtime, repairs,
clean-out, and lost production. Corrective action would
be either a replacement of the uid or a major dilution
with virgin uid to maintain uid properties within
normal range.
Venting
Since the expansion tank is usually installed
at a high point in the system, it also can serve
as the main venting point of the system for
excess levels of low boilers and moisture which
may accumulate in the heat transfer uid.
To properly vent a heat transfer uid system,
the expansion tank must be capable of
accommodating the circulating ow of hot
heat transfer uid. To remove low boilers, the
temperature in the expansion tank will be
increased and the tank pressure may be
lowered while venting. As they ash into the
vapor space, the excess low boilers and
moisture can be more effectively removed by
sweeping out the expansion tank through the
vent line to a safe area (preferably via a cooled
condenser). Modest pressure decreases help
minimize the loss of good heat transfer uid in
the vent stream.
9
Property Possible cause Potential effects Suggested limit
Viscosity changes
Contamination, thermal degradation,
uid oxidation
Poor heat transfer rate, deposits, high
vapor pressure, pump cavitation
Depends on uid chemistry
Moisture increase
System leaks, residue in new or cleaned
unit, unprotected vent or storage
Corrosion, excess system pressure,
pump cavitation
700 ppm (for heating service)
Flash point decrease
Contamination,
high amount of low boiler
Increased re hazard, change
of regulatory requirements
Jurisdictional requirements
Total acid number increase
Severe oxidation,
contamination with acid
System corrosion, deposits 0.7 mg KOH/g
Insoluble solids increase
Contamination, dirt, corrosion,
oxidation, thermal stress
Poor heat transfer, wear of pump seals,
plugging of narrow passages
400 mg/100 mL
Low boiler (LB) and high
boiler (HB) increase
Contamination, thermal stress
Pump cavitation, poor heat transfer,
excess system pressure, deposits
5% (LB)
10% (HB)
Summary
Changes in uid properties are often the result of
thermal and oxidative degradation. Depending on the
stability of the particular heat transfer uid used, all
actions previously described to maintain uid properties
may have to be considered on a regular basis. It has to
be acknowledged that all organic heat transfer uids
will degrade. The key differences among uids are their
respective rates of degradation under operating conditions
and the nature of the degradation products formed.
Selection of the proper heat transfer uid, having adequate
thermal stability along with good system design and
operation, can optimize uid life and performance while
helping maintain high system reliability.
10
Table 1Summary of in-use heat transfer uid test results: Interpretation.
About the authors
Conrad Gamble, P.E. is the product steward for Therminol
heat transfer uids at Solutia Inc., a subsidiary of Eastman
Chemical Company and is based in Anniston, Ala., U.S.A.
Phone: 256-231-8525
Email: [email protected]
He currently supports the Therminol business in product
development and customer technical support and
provides customer educational training. He joined Solutia
Inc. (then Monsanto Co.) in 1985 as a process engineer.
He has advanced in various manufacturing and engineering
roles until his current assignment as technical service
associate. A licensed professional engineer and recognized
expert in the industry, Gamble has served the chemical
industry for more than 25 years. He is also a member of
the American Institute of Chemical Engineers. Gamble
holds a BS in Chemical Engineering from the University
of Alabama, Tuscaloosa, Ala.
Matthias Schopf is the Technical Service Manager of
Eastmans Specialty Fluids business in Europe (Solutia
Europe BVBA/SPRL, a subsidiary of Eastman Chemical
Company).
Phone: +32-2-746-5195
Email: [email protected]
His responsibilities include providing technical service to
Therminol heat transfer uid customers as well as
leading activities in new technologies like renewable
energy production. Prior to this role, he worked as Sales
Engineer for heat transfer uids and aviation hydraulic
uids in Europe and Middle East for more than 10 years.
Before joining Solutia in 1996, he worked as an Engineer
for Machine Monitoring Systems for power plants and in
low-temperature thermometry research at the German
institute PTB. He received an MSc degree in Physics in
1989 from Humboldt University in Berlin, Germany.
References
i ASTM D6743-11, Standard Test Method for Thermal
Stability of Organic Heat Transfer Fluids, 2011, ASTM
International, Conshohocken, Pa. 19428-2959, U.S.A.
ii DIN 51528:1998-07, Testing of mineral oils and
related productsDetermination of thermostability
of unused heat transfer uids.
iii Therminol Information Bulletin No. 6, Heat Transfer
Fluid Maximum Temperature Ratings, Pub. No.
7239686 rev. A, Solutia Inc., subsidiary of Eastman
Chemical Company.
iv Liquid Phase Systems Design Guide, TF-04 5/14, pg. 16,
Solutia Inc., subsidiary of Eastman Chemical Company.
v ASTM D445-12, Standard Test Method for Kinematic
Viscosity of Transparent and Opaque Liquids (and
Calculation of Dynamic Viscosity), 2012, ASTM
International, Conshohocken, Pa. 19428-2959, U.S.A.
vi ASTM E203-08, Standard Test Method for Water
Using Volumetric Karl Fischer Titration, 2008, ASTM
International, Conshohocken, Pa. 19428-2959, U.S.A.
vii ASTM D92-12b, Standard Test Method for Flash and
Fire Points by Cleveland Open Cup Tester, 2012,
ASTM International, Conshohocken, Pa. 19428-2959,
U.S.A.
viii

ASTM D93-13e1, Standard Test Methods for Flash
Point by Pensky-Martens Closed Cup Tester, 2013,
ASTM International, Conshohocken, Pa. 19428-2959,
U.S.A.
ix ASTM D664-11-a, Standard Test Method for Acid
Number or Petroleum Products by Potentiometric
Titration, 2011, ASTM International, Conshohocken,
Pa. 19428-2959, U.S.A.
x Therminol Information Bulletin No. 2, In-Use Testing
of Therminol Heat Transfer Fluids, Pub. No. 7239112C.
11
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Safety Data Sheets providing safety precautions that should be observed
when handling and storing our products are available online or by request.
You should obtain and review available material safety information before
handling our products. If any materials mentioned are not our products,
appropriate industrial hygiene and other safety precautions recommended
by their manufacturers should be observed.
2014 Eastman Chemical Company. Eastman, The results of insight, and
Therminol are trademarks of Eastman Chemical Company or one of its
subsidiaries. The used herein denotes registered trademark status in the
U.S.; marks referenced herein may also be registered internationally.
TF-50 10/14