Feature Report

Part 2

ASTM Standards For

Fleat Transfer Fluids
This practical overview of ASTM standards can serve as a roadmap
when selecting and evaluating heat transfer fluids
Gerald E. Guffey II on equipment, efficiency (heat-trans­
Eastman Chemical Co. fer capability) and service life.
eat-transfer-fluid systems Pumpability. Several properties are

H
are often used for pro­ relevant to the pumpability of a heat
cess heating to 500°F transfer fluid. Pumpability is briefly
or higher. To accomplish discussed in this standard, but it is
heating above 500°F, steam pres­ discussed more extensively in D8046.
sure must be above 600 psig. For Decreased flash point (measured by
many plants, distributing steam D92 or D93) is indicative of the pres­
above 600 psig is impractical due ence of low-boiling compounds pro­
to high cost and more stringent wa­ duced by thermal degradation of the
ter-purity requirements. High-tem- fluid. Viscosity (measured by D445 or
perature heat-transfer fluids have D7042) is a measurement of the flu­
a much lower vapor pressure than id's resistance to flow. The presence
water at high temperature, so the of thermal degradation products can
design pressure of a heat-transfer- affect the viscosity of the fluid. As fluid
fluid system can be lower. temperature is decreased, at some
Most systems operate with the point the fluid viscosity becomes too
heat transfer fluid in the liquid phase. high to pump. There is some correla­
A few heat transfer fluids have a tion between hydraulic shock during
FIGURE 1. One type ot synthetic organic heat
narrow boiling range and can be transfer fluid is shown here pumping with the fluid’s specific grav­
used in a vapor-phase system, but ity (measured by D1298 or D4052)
the design of the system is much transfer fluids other than inorganic and compressibility properties. Water
different and the process heating eutectic salts. This article provides an in a heat-transfer-fluid system will va­
temperature must match the boiling overview of these standards. ASTM porize and expand as system tem­
range of the fluid. standards are listed using their ASTM perature is increased, building pres­
High-temperature heat-transfer designations, for example D5372. sure. It is therefore important to keep
fluids are generally classified as inor­ “D” indicates that the standard is water out of the system as much as
ganic eutectic salts, synthetic organ­ administered by one of the D com­ possible. Water content can be mea­
ics (Figure 1), aromatic oils, paraffinic mittees. “5372” is the number of the sured using D95.
oils and silicone-based fluids. The standard. These designations are Safety. Factors related to safety in
chemistry of each heat-transfer fluid used throughout this article. use include autoignition temperature
is different, so each fluid has differ­ and flashpoint. Autoignition temper­
ent properties. Considerable back­ ASTM D5372 standard guide ature can be measured using E659.
ground and technical information ASTM D5372, “Standard Guide for The user should keep in mind that
about heat transfer fluids is provided Evaluation of Hydrocarbon Heat a hydrocarbon fluid absorbed on a
in chapter 21 of the ASTM Fuels and Transfer Fluids,” covers the factors porous inert surface (such as insula­
Lubricants Handbook. A new version that should be considered to char­ tion) can ignite at temperatures more
of this handbook is expected to be acterize a heat transfer fluid. These than 50°C lower than the value de­
published this month. factors are also relevant to selection termined by E659. Flashpoint (mea­
ASTM International (formerly of a new heat-transfer fluid, so it can sured by D92 Cleveland open cup
known as the American Society for be used as a reference when choos­ tester or D93 Pensky-Martens closed
Testing and Materials; West Con- ing a new fluid. These factors are cup tester) indicates the temperature
shohocken, Pa.; www.astm.org) has grouped into five categories: pump- at which flammable vapors given off
developed several standards for heat ability of the fluid, safety in use, effect by a liquid form a mixture with air that

48 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2019

can be ignited by contact with a hot
surface, spark, or flame.
Effect on equipment. Two ASTM
standards can provide information
about the effect of the heat transfer
fluid on equipment. D471 provides
data about the effect of the fluid on
rubber or elastomeric seals. G4 is a
guide for conducting corrosion tests in
field applications.
Efficiency. Several properties —
thermal conductivity, specific heat,
density and viscosity — are relevant
to the heat transfer capability of the
fluid. These are the properties used to
calculate Reynolds number, Prandtl
number and Nusselt number, which
determine the heat transfer coeffi­
cient. D2717 measures thermal con­
ductivity, D1298 or D4052 measures
specific gravity, and D445 or D7042
measures viscosity. D2766, the test
method listed for specific heat, has
recently been withdrawn but E1269
and E2716 are other methods that
could be considered.
Service life. Heat transfer fluids de­
grade when exposed to sufficiently
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high temperature. The amount of
degradation increases as tempera­
ture increases or exposure time
increases. Thermal stability is mea­
sured using D6743.
Several tests are used to deter­
mine the condition of the fluid and
its remaining service life. These
tests include precipitation number
(measured by D91), insoluble con­
tent (measured by D893), flash point
(measured by D92 or D93), carbon
residue (measured by D189, D524
or D4530), distillation (D86, D1160
and D2887 are listed but D2887 is
more commonly used), neutralization
number (measured by D664), color
(measured by D1500), viscosity, vis­
cosity index (measured by D2270)
and water content (measured by
D95). Typically, a sample of used
heat-transfer fluid should be taken
from each system at least once per
year so that these tests can be con­
ducted to evaluate fluid condition.
To ensure that the sample is repre­
sentative, it should be taken from
the main circulating loop rather than
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fluid suppliers offer free evaluation of
used fluid using these tests.
ASTM D7665 standard guide
ASTM D7665, “Standard Guide for
Evaluation of Biodegradable Heat
Transfer Fluids,” addresses biode­
gradable heat transfer fluids. It cov­
ers the same factors mentioned in
D5372 but also includes a few oth­
ers. Vapor pressure (measured by
D2879) is included as a factor that in­
fluences pumpability of the fluid. Bio­
degradation (measured by D5864) is
included as a factor to consider for
safety in use. D6384, which covers
terminology related to biodegrad­
ability and ecotoxicity of lubricants,
is listed as a reference document.
D7044, which is a specification for
biodegradable fire-resistant hydrau­
lic fluids, is also listed as a reference.
ASTM D6743 standard test method
ASTM D6743, “Standard Test
Method for Thermal Stability of Or­
ganic Heat Transfer Fluids," is a
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test method that measures ther­
mal stability of a heat transfer fluid.
Thermal stability is the resistance to
permanent change in fluid proper­
ties caused solely by heat. All heat-
transfer fluids degrade with expo­
sure to high temperature over time.
Typically, the user wants their heat
transfer fluid to last for many years.
It’s important to select a fluid that is
thermally stable enough to last for
many years at the expected system
operating temperature.
The thermal degradation products
for most heat transfer fluids include
high- and low-boiling components,
very low-boiling gases, and residue
that cannot be evaporated. The
presence of degradation products in
the fluid affects its properties.
D6743 quantifies the high-boiling
components, low-boiling compo­
nents, very low-boiling gases, and
residue that cannot be evaporated
for a heat transfer fluid that is ex­
posed to specified temperature for
a specified time period. The test
procedure consists of weighing heat
transfer fluid into a stainless-steel
ampoule, purging with nitrogen,
sealing the ampoule, and heating
it in an oven. After the ampoule is
removed from the oven and cooled,
the fluid is analyzed to quantify the
amount of thermal degradation
products produced. Measurement
of thermal degradation products is
done by gas chromatography (GC),
distillation and weighing.
Before D6743 was developed,
each heat-transfer-fluid manufac­
turer had its own method for deter­
mining thermal stability. There were
differences in the methods, as well
as differences in the equipment used
to conduct them. These differences
sometimes led to conflicting test re­
sults. One supplier’s test data might
indicate that fluid A was more ther­
mally stable than fluid B, while an­
other supplier’s test data might show
the opposite.
D6743 provides a standard test
method for developing data that a
user can evaluate to compare heat
transfer fluids. Using D6743, ther­
mal stability of two or more different
heat-transfer-fluid chemistries can
be directly compared by heating
them at the same time in the same
oven, and then analyzing them
using the same equipment. D6743
is very specific about the type of
equipment that can be used. For
example, it specifies the type and
length of the GC column, film type
and thickness, type of detector,
calibrant range, material and dimen­
sions of the ampoule, temperature
control capability of the oven, and
accuracy of the balance for weigh­
ing. Statistical analysis of test data
from one laboratory showed very
good repeatability of test results
(see the precision and bias state­
ment in the method).
DIN (Deutsches Institute fur Nor-
mung e.V.; Berlin, Germany; www.
din.de) also has a test method for
thermal stability, but it is less specific
about the test equipment that can be
used. Differences in test equipment
used can cause significant differ­
ences in test results.

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 LIST OF ASTM STANDARDS REFERENCED IN THIS ARTICLE
D5372 Standard Guide for Evaluation of Hydrocarbon Heat Trans­
fer Fluids
D93 Standard Test Methods for Flash Point by Pensky-Martens
Closed Cup Tester
D445 Standard Test Method for Kinematic Viscosity of Transpar­
ent and Opaque Liquids (and Calculation of Dynamic Vis­
cosity)
D7042 Standard Test Method for Dynamic Viscosity and Density
of Liquids by Stabinger Viscometer (and the Calculation of
Kinematic Viscosity)
D1298 Standard Test Method for Density, Relative Density, or API
Gravity of Crude Petroleum and Liquid Petroleum Products
by Hydrometer Method
D4052 Standard Test Method for Density. Relative Density, and API
Gravity of Liquids by Digital Density Meter
D95 Standard Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation
E659 Standard Test Method for Autoignition Temperature of
Chemicals
D92 Standard Test Method for Flash and Fire Points by Cleve­
land Open Cup Tester
D471 Standard Test Method for Rubber Property-Effect of Liq­
uids
G4 Standard Guide for Conducting Corrosion Tests in Field Ap­
plications
D2717 Standard Test Method for Thermal Conductivity of Liquids
D6743 Standard Test Method for Thermal Stability of Organic Heat
Transfer Fluids
D91 Standard Test Method for Precipitation Number of Lubri­
cating Oils
D893 Standard Test Method for Insolubles in Used Lubricating
Oils
D189 Standard Test Method for Conradson Carbon Residue of
Petroleum Products
D524 Standard Test Method for Ramsbottom Carbon Residue of
Petroleum Products
D4530 Standard Test Method for Determination of Carbon Resi­
due (Micro Method)
D86 Standard Test Method for Distillation of Petroleum Products
and Liquid Fuels at Atmospheric Pressure
D1160 Standard Test Method for Distillation of Petroleum Products
at Reduced Pressure
D2887 Standard Test Method for Boiling Range Distribution of Pe­
troleum Fractions by Gas Chromatography
D664 Standard Test Method for Acid Number of Petroleum Prod­
ucts by Potentiometric Titration
D1500 Standard Test Method for ASTM Color of Petroleum Prod­
ucts (ASTM Color Scale)
D2270 Standard Practice for Calculating Viscosity Index from Ki­
nematic Viscosity at 40 °C and 100°C
D7665 Standard Guide for Evaluation of Biodegradable Heat
Transfer Fluids
D2879 Standard Test Method for Vapor Pressure-Temperature Re­
lationship and Initial Decomposition Temperature of Liquids
by Isoteniscope
D5864 Standard Test Method for Determining Aerobic Aquatic
Biodegradation of Lubricants or Their Components
D6384 Standard Terminology Relating to Biodegradability and
Ecotoxicity of Lubricants
D7044 Standard Specification for Biodegradable Fire Resistant
Hydraulic Fluids
D7863 Standard Guide for Evaluation of Convective Heat Transfer
Coefficient of Liquids
D8046 Standard Guide for Pumpability of Heat Transfer Fluids
E794 Standard Test Method for Melting And Crystallization Tem­
peratures By Thermal Analysis
D2983 Standard Test Method for Low-Temperature Viscosity of
Automatic Transmission Fluids. Hydraulic Fluids, and Lubri­
cants using a Rotational Viscometer
D891 Standard Test Methods for Specific Gravity, Apparent, of
Liquid Industrial Chemicals
D6304 Standard Test Method for Determination of Water in Petro­
leum Products, Lubricating Oils, and Additives by Coulo-
metric Karl Fischer Titration

ASTM D7863 standard guide
ASTM D7863, “Standard Guide for
Evaluation of Convective Heat Trans­
fer Coefficient of Liquids," provides
information about the calculation of
convective heat-transfer coefficient.
The factors that affect calculation of
convective heat-transfer coefficient
are described. Results from previ­
ous studies have been presented in
different ways, so direct comparison
of convective heat-transfer-coeffi-
cient data from these studies can
be challenging. Therefore, this guide
focuses on describing a standard
approach for obtaining data, inter­
preting data, and presenting results.
This guide describes a test equip­
ment arrangement with turbu­
lent fluid flow inside an electrically
heated tube that has a wall tem­
perature higher than the bulk fluid
temperature. Features of this test-
equipment arrangement are dis­
cussed and the required measure­
ments are defined. The ASTM test
methods recommended for mak­
ing each of the required measure­
ments are listed. Considerations for
calibration of the test equipment are
discussed. Formulas used to cal­
culate the heat-transfer coefficient
are summarized. Appropriate ways
to interpret, present and report the
test results are explained.
ASTM D8046 standard guide
ASTM D8046, “Standard Guide for
Pumpability of Heat Transfer Flu­
ids,” discusses the fluid properties
and system configuration issues
that affect the ability to pump a heat
transfer fluid. These properties in­
clude flashpoint (measured by D92
or D93), crystallization temperature
(measured by E794), viscosity (mea­
sured by D445, D2983 or D7042),
relative density (measured by D891
or D4052), water content (measured
by D6304), vapor pressure (mea­
sured by D2879), and boiling range
distribution (measured by D2887).
System configuration issues include
the type of pump used, mechanical
seals, the pump suction piping ar­
rangement, net positive-suction head
required by the pump, and electric
motor sizing. The need to consider
how fluid viscosity will change as the
fluid degrades and how that affects
pump and motor selection is also
discussed. This guide addresses
several considerations about pump­
ing that are a useful reference when
selecting a new heat-transfer fluid.!
Edited by Gerald Ondrey
Author
Gerald Guffey Is a senior associ­
ate engineer in the Worldwide En­
gineering and Construction Divi­
sion ol Eastman Chemical Co.
(t 00 Eastman Road, Kingsport. TN
37660; Phone; 423-229-1095;
Email: ggutfey@eastman.com).
He has been involved in design
and evaluation of heat transfer
fluid systems and fired heaters for
more than twenty years. He has been a member of
ASTM since 1997. He holds a Bachelor of Science de­
gree in Mechanical Engineering from Georgia Tech.

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