Heat Transfer Fluids

Understanding and maintaining petroleum heat transfer

fluids and their systems

Rev. 2

April 10, 2007

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 Heat Transfer Fluids
1. INTRODUCTION .................................................................................................................................. 4
2. THEORY............................................................................................................................................... 5
2.1. WHAT IS A HEAT TRANSFER SYSTEM?.............................................................................................. 5
3. REQUIREMENTS OF HEAT-TRANSFER FLUIDS............................................................................. 6
3.1. CHEMICALLY STABLE ...................................................................................................................... 6
3.2. GOOD HEAT TRANSFER CHARACTERISTICS ...................................................................................... 6
3.3. LOW VOLATILITY ............................................................................................................................. 6
3.4. ENSURES ADEQUATE FLOW RATES .................................................................................................. 7
3.5. NON-CORROSIVE AND NON-TOXIC ................................................................................................... 7
3.6. WATER AS A HEAT TRANSFER FLUID ................................................................................................ 7
3.7. PETROLEUM OILS AS HEAT TRANSFER FLUIDS .................................................................................. 8
4. DEGRADATION OF PETROLEUM HEAT TRANSFER FLUIDS ....................................................... 9
4.1. THERMAL CRACKING ....................................................................................................................... 9
4.2. OXIDATION................................................................................................................................... 12
5. HEAT TRANSFER SYSTEM DESIGN .............................................................................................. 13
5.1. OPEN OR CLOSED SYSTEM ............................................................................................................ 13
5.2. HEATING UNIT .............................................................................................................................. 14
5.3. PUMPS ........................................................................................................................................ 15
5.4. FILTERS ....................................................................................................................................... 15
5.5. PROCESS VESSEL - USER ............................................................................................................. 16
5.6. EXPANSION TANK ......................................................................................................................... 16
6. HEAT TRANSFER SYSTEM OPERATION....................................................................................... 18
6.1. INITIAL FILLING ............................................................................................................................. 18
6.2. START-UP .................................................................................................................................... 19
6.3. REGULAR OPERATION .................................................................................................................. 20
6.4. WATER CONTAMINATION IN HEAT TRANSFER FLUIDS ....................................................................... 20
6.5. FLUSHING .................................................................................................................................... 22
6.6. SYSTEM MAINTENANCE ................................................................................................................ 23
7. SAFETY ............................................................................................................................................. 24
7.1. OPERATOR TRAINING ................................................................................................................... 24
7.2. FIRE PREVENTION ........................................................................................................................ 25
8. OIL LIFE - USED OIL ANALYSIS ..................................................................................................... 27
8.1. SAMPLING PROCEDURES .............................................................................................................. 28
8.2. TYPICAL ANALYSIS ....................................................................................................................... 30
8.3. KINEMATIC VISCOSITY (KV) .......................................................................................................... 30
8.4. TOTAL ACID NUMBER (TAN)......................................................................................................... 31
8.5. WATER ........................................................................................................................................ 31
8.6. SEDIMENT.................................................................................................................................... 32
8.7. METALS (ICPES)......................................................................................................................... 33
8.8. FLASH POINT................................................................................................................................ 34
8.9. SIMULATED DISTILLATION BY GAS CHROMATOGRAPHY (GCD) ....................................................... 36
9. TROUBLESHOOTING HEAT TRANSFER SYSTEMS ..................................................................... 38
9.1. THE VICIOUS CIRCLE OF HEAT TRANSFER FLUID DEGRADATION........................................................ 38
9.2. IDENTIFYING ROOT CAUSES........................................................................................................... 39
9.3. COMMON SYMPTOMS AND CAUSES ................................................................................................ 39
10. CONCLUSION ............................................................................................................................... 43

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Summary
This technical bulletin is a collection of current information related to circulating oil heat
transfer systems, including:
• principles of heat transfer,
• design of typical industrial heat transfer systems,
• properties of heat transfer fluids,
• heat transfer system maintenance,
• used heat transfer oil analysis, and
• heat transfer system troubleshooting.

This bulletin is destined for users of industrial circulating oil heat transfer system as well
as individuals involved in the marketing and technical support of these systems and
heat transfer fluids.

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1. Introduction
Fluid heat transfer systems are known by a variety of names: thermal fluid systems, hot
oil systems, thermal liquid systems, thermal oil heat-transfer systems and variations on
these. However, all these terms refer to industrial heating systems where a special
thermal fluid is re-circulated by a pump through a heater (or heaters) thereby raising the
temperature of the fluid which is then used in heating various processes.

Typical applications include:

• Heating press platens such as laminating presses used in particleboard and/or
waferboard manufacturing
• Supplying heat for rubber and plastics moulding, extrusion, curing and
calendering
• Heating chemical, petrochemical and other process equipment such as reactors,
heat exchangers, dryers and evaporators
• Lumber drying
• Paper and paperboard products
• Printing; speed roll heating
• Varnish and resin formulations

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2. Theory
KEY POINTS:
9 A heat transfer system is one designed to transfer heat from one source to another.
9 There are two main types of heat transfer systems: DIRECT (with contact) and INDIRECT (such
as using a fluid)

DIRECT heat transfer

9 Fine control of heat transfer is difficult

INDIRECT heat transfer is preferred

9 It is possible to maintain close control of the transfer of heat to a number of processes or
areas from one primary heating unit
9 The heating unit can be remote from the process and be located in the most convenient place

2.1. What is a heat transfer system?

A heat transfer system is one that has been designed to transfer heat from one source
to another. Heat transfer systems can be divided into two large categories: direct heat
transfer systems and indirect heat transfer systems

Direct heat transfer is heating or cooling applied directly to the item being heated. An
example is the heating of a kettle on a stove.

Indirect heat transfer uses an intermediate fluid to carry heat from the source to the
receiver. A common example of an indirect heat transfer system is the central heating
system in a home or office where water, steam or air is the heat-transfer medium. Heat
transfer systems using circulating oil are also examples of indirect heat transfer
systems.

The advantages of indirect heating systems are:

1. Closer control of heat output. The heat transfer fluid can be used to smooth out
the variation of the output of the heat source.
2. The heat source can be separated from the material being heated. This is
important where the material being heated is very flammable.
3. More even heat distribution can be obtained
4. No overheating
5. Heat can be supplied to a number of areas from one primary heating unit

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3. Requirements of heat-transfer fluids
SUMMARY OF REQUIRED HEAT TRANSFER FLUID CHARACTERISTICS:

Basic requirements:
9 Stability at high operating temperatures: resist oxidation and thermal cracking
9 Good heat transfer characteristics: high specific heat and high thermal conductivity
9 Low vapour pressure to prevent vapour lock/cavitation at the pump
9 Low safety risk: high flash and fire point
9 Low viscosity, to decrease pumping losses, and a high viscosity index to reduce variation in
loads on equipment
9 Non-corrosive and non-toxic

Petroleum oils as heat transfer fluids:

9 By far the most widely used heat transfer fluid for systems operating up to 316ºC (600 ºF).
9 Offer advantages over other fluids: wide availability, low cost, good thermodynamic
properties, long life and ease of handling.

Effective heat-transfer fluids must have a number of desired properties.

3.1. Chemically stable

Heat transfer fluids must resist deterioration at the temperatures they operate; this is
known as thermal stability. In the case of petroleum oils, the fluid must also resist
breakdown due to exposure to oxygen, also called oxidation stability.

3.2. Good heat transfer characteristics

Heat transfer fluids must possess good heat-transfer characteristics; specifically they
must have high specific heat and high thermal conductivity.

¾ Specific heat of a material is the amount of heat required to raise the temperature
of 1 gram of the material through 1°C. It is a measure of a material’s heat
capacity, which is its ability to store heat as it changes in temperature. Materials
such as metals require very little energy to increase their temperature and
therefore do not store this heat very effectively; these are materials with low
specific heat. Water is an example of a material with high specific heat as it
requires a large amount of energy to increase its temperature and will preserve
this heat relatively well.

¾ Thermal conductivity is a measure of a material's ability to conduct heat, or

transfer heat, through direct physical contact. High thermal conductivity will allow
for rapid heat transfer.

3.3. Low volatility

It is important that heat transfer fluids have low vapour pressures at operating
temperatures:
• to prevent vapour lock and cavitation at the pump,
• minimize losses in open systems, and

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 • eliminate the need for high pressure piping.

¾ Vapour pressure is a measure used to describe a liquid's tendency to evaporate.

It is the pressure, at a given temperature, at which a fluid's tendency to evaporate
and its tendency to condense are in equilibrium. A material with a high vapour
pressure at ambient temperatures is often referred to as a volatile material (in
other words, it requires high pressure to keep it from evaporating). The higher
the vapour pressure of a material at a given temperature, the lower the boiling
point.

The fluid must present a low fire risk by having a high flash and fire point.

¾ The flash point of an oil is the temperature at which the oil releases enough
vapour at its surface to ignite momentarily when an open flame is applied.
¾ The fire point is the temperature at which vapours are released rapidly enough to
support sustained combustion.

3.4. Ensures adequate flow rates

In terms of viscometric properties, the fluid should have low viscosity, to decrease
pumping losses and to reduce the power required for circulation. Furthermore, low
viscosity fluids encourage turbulent flow which promotes efficient heat transfer. The
fluid should also have a high viscosity index to reduce variation in loads on equipment
and similarly a low pour point to avoid cold starting difficulties where applicable.

Although recommended practise is to separate the lubricating oil of the pump from the
heat transfer oil, this is rarely implemented in heat transfer system design. In fact, heat
transfer oils are frequently used to lubricate system pumps. Therefore, the choice of
fluid viscosity becomes a balance between ensuring turbulent flow, adequate circulation
and pump lubrication.
¾ Viscosity is a measure of a fluid's resistance to flow, or, in simpler terms, a
measure of a fluid's thickness. The thicker the liquid, the higher the viscosity.
¾ Viscosity Index (Vl) measures the rate at which the viscosity of an oil will change
as the temperature changes. The higher the VI, the less the viscosity changes
with temperature.

3.5. Non-corrosive and non-toxic

The fluid must protect system components against corrosion and be easy to handle in
the sense that it is non-toxic.

3.6. Water as a heat transfer fluid

Water and steam are excellent heat-transfer media. Water has a high specific heat and
steam has a high latent heat. They do not deteriorate with use and are low in cost.
However, they will rust piping and other ferrous parts. Since steam pressure increases
very rapidly as operating temperature increases, these high temperatures require
expensive high-pressure equipment. This requires condensate return systems,

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treatment of boiler water to protect against scale and may even require a licensed
operator. None of these is necessary when using petroleum oil.

3.7. Petroleum oils as heat transfer fluids

There are a variety of heat transfer fluids available in the market place, from petroleum
(mineral and synthetic) to other chemical basestocks. However, petroleum oils are by
far the most popular and widely used heat transfer media for systems operating up to
316ºC (600 ºF). They offer advantages over other fluids because of their wide
availability, low cost, good thermodynamic properties, long life and ease of handling.

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4. Degradation of petroleum heat transfer fluids
SUMMARY OF HEAT TRANSFER OIL DEGRADATION:

Thermal Cracking:
9 Occurs with all hydrocarbon fluids at oil temperatures above 360°C (680°F)
9 Forms light relatively volatile products (low-boilers), some of which combine into heavier
products (high boilers)
9 Characterized by insolubles and coke formation and a decrease in oil viscosity and flash point
9 The thin film of oil closest to piping walls is most susceptible to thermal cracking due to its
lower speed

Oxidation:
9 Only occurs if air or oxygen is present.
9 Oxidation can be a relatively rapid process at high temperatures characterized by viscosity
increase, sludge and deposit formation and acid build-up

In both cases, heat transfer properties of the oil are negatively affected:
9 Build-up on heat exchanger walls interferes with heat exchange and can promote further
thermal cracking by creating hot spots within the system, or increase laminar flow through
pipe constriction

4.1. Thermal cracking

Not all petroleum fluids are suitable as heat transfer fluids. When typical petroleum
fluids are exposed to high temperatures, some of the carbon-hydrogen bonds break and
form new materials. This thermal cracking occurs in the absence of oxygen.

Thermal cracking forms:

• light, relatively volatile products, also known as low-boilers. These lighter
products can cause pump cavitation and decrease the flash point of the fluid,
potentially posing a fire hazard.
• Some of the light products may polymerize (combine) into heavier, more viscous
products, sometimes called high boilers. These heavier products can increase
the resistance of fluid flow through the system, putting strain on the system
pumps. Furthermore, these can lead to the deposition of coke-like materials on
heat transfer surfaces creating hot spots in a system, which accelerate the
cracking process.

Resistance to thermal cracking varies with the structure and refining techniques used to
produce a petroleum oil. Thermal cracking will occur with all hydrocarbon fluids at oil
temperatures above 360°C (680°F). At these temperatures, the thermal vibration
causes splitting of the carbon-carbon bonds. Linear paraffins are most susceptible to
cracking because they have single carbon-carbon bonds. Aromatic hydrocarbons are
the most stable because the double carbon-carbon bonds require more energy to break.

It is important to note that hydrocarbon fluids are typically a mixture of many different
hydrocarbon structures. Within this mixture are less stable hydrocarbon molecules
which will breakdown at temperatures below the recommended maximum bulk oil

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temperature. The breakdown of these molecules will in turn create catalysts for further
degradation.

The bond strength and recommended bulk oil temperatures for different hydrocarbon
chemical structures are displayed in Figure 1.

Figure 1, Thermal stability of hydrocarbon structures

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 4.1.1. Film Temperatures
In the operation of any heat transfer system, a wide range of fluid temperatures exists
between the hottest and coolest areas. Under conditions of laminar flow, such as in
Figure 2, where all the fluid is traveling in the same direction, there is a layer of fluid
next to the wall of the heating tube or coil that is distinct from the main stream.
Figure 2, Fluid velocity under laminar
This outermost layer (also called a film)
FLUID VELOCITY
clings to the tube wall and flows more
slowly than the rest of the fluid. Its slower
speed and its proximity to the heat source
can cause the temperature of this layer
to be much higher than the bulk
temperature. If the difference is great

TUBE WALL
TUBE WALL
enough, the film temperature may
exceed the maximum recommended
bulk temperature of the fluid.

The difference between the film

temperature and bulk temperature
depends primarily on flow velocity and
flow turbulence.
• Flow velocity: The faster the flow
velocity, the thinner the film clinging to the tube wall.
• Flow turbulence: Turbulent flow, where layers of fluid within a fluid stream travel
in many different directions, reduces the fluid film subjected to overheating.
Laminar flow, where all the fluid travels in the same direction, increases the film
thickness.

Figure 3 illustrates typical heat transfer Figure 3, Typical heat transfer oil temperature
oil temperature design considerations.
Knowing that rapid oil decomposition 360°C RAPID OIL DECOMPOSITION
occurs above 360°C (680°F), a 20°C
(68°F) safety allowance is 20°C SAFETY
TEMPERATURE
TUBE WALL

recommended for the maximum oil film ALLOWANCE

temperature adjacent to a heat source.

HEAT

A 25°C (77°F) temperature difference 340°C MAX FILM TEMP

between the bulk oil temperature and

the film temperature is typical in well FLUID 25°C OIL FILM
ALLOWANCE
designed heat transfer systems.
Therefore, an operating limit of 315°C
315°C MAX BULK TEMP
(600°F) for the bulk oil temperature
would generally ensure minimum oil
degradation due to thermal stress.

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The flow characteristics of a heat transfer system are dependent upon the design of the
system, the viscosity of the fluid and the in-service condition of the system and the fluid.

As a system ages and is allowed to become dirty, deposits can constrict fluid
passages, which promotes laminar flow. These same deposits can also insulate
heat transfer surfaces thus creating hotspots elsewhere. Therefore it is very
common for a system that previously did not have film temperatures that
exceeded the oil's thermal limits to begin to exhibit the symptoms of thermal
degradation.
*Note: Turbulence can be estimated by calculating the Reynolds number for a system, which is a ratio of
inertial forces to viscous forces within the moving fluid. The Reynolds number (Re) equation, for flow
through a cylindrical pipe, is:
υs L
Re = where:
ν
υs - mean fluid velocity, m/s
L - characteristic dimension, m (= diameter of pipe)
ν - kinematic fluid viscosity, m2/s (1 cSt = 10-6 m2/s)

Laminar flow occurs at low Reynolds numbers, where viscous forces are dominant, while turbulent flow
occurs at high Reynolds numbers and is dominated by inertial forces. The transition between laminar and
turbulent flow is gradual. Within circular pipes, the transition Reynolds number is generally accepted to
be 2300, but system designers will choose a pipe configuration that falls either below approximately 2000
to ensure that the flow is laminar or above 4000 to ensure that the flow is turbulent.

4.2. Oxidation
Oxidation is the term used to describe the chemical reaction that occurs between oil and
oxygen in the presence of heat or light producing unstable reactive compounds. The
rate of this reaction increases as temperature increases, generally doubling for every
10°C increase over 70°C. Therefore, oil exposed to air at high temperatures, such as in
a heat transfer system, can oxidize at a relatively rapid rate.

Oxidation leads to the formation of organic acids and sludges that are often compared
to (and referred to as) resins/varnishes. These resulting by-products thicken the oil and
eventually form insoluble material that deposit on heaters and other surfaces of the
system. The by-products of oxidation tend to act as a catalyst for further oxidation.
These coke-like deposits have an insulating effect on the system thus interfering with
heat transfer. This creates the need for higher heater temperatures that can thermally
degrade the oil and/or rupture system piping.

Properly formulated heat transfer oils should provide excellent oxidation stability through
a combination of base stock selection and additive treatment, including oxidation
inhibitors. The oil should also contain additives that will help control deposit formation
and keep sludge in solution so that is does not drop out and create deposits.

Oxidation problems can be virtually eliminated by the exclusion of air, such as through
the installation of an inert gas blanket in the expansion tank. Oxidation can also be
slowed by lowering expansion tank temperatures.

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5. Heat Transfer System Design
SUMMARY OF HEAT TRANSFER SYSTEM DESIGN:
9 Two basic types of systems: Open and Closed

OPEN systems:
9 Expansion tank vented to the atmosphere. Allows for air entry and increased oil oxidation
CLOSED systems:
9 Expansion tank sealed from atmosphere with nitrogen blanketing and/or expansion bellows.
9 Greatly reduces oil oxidation

TYPICAL COMPONENTS:
9 HEATER: Design and operation are critical to managing thermal stress on fluid:
Temperatures should not exceed 360°C.
Heat input of electrical heaters should be less than 2.6 W/cm2.
Direct flame impingement must be avoided.
9 PUMPS: Must be suitable for high temperature service and maintain a flow rate to provide
required heat for users and minimize thermal stress on fluid.
9 FILTERS: Effective filtration is essential for trouble free operation and promoting long fluid
and system life
9 EXPANSION TANK: Critical to safe system performance by accommodating oil expansion and
managing oxidation by limiting contact between hot oil and air

There are many variations in the design of circulating oil heat transfer systems.
However, certain features are common to all and these are illustrated in Figure 4.

The essential components of a heat transfer system are the following:

1. Heating unit
2. Circulating pump
3. Filter
4. Process vessel
5. Expansion tank or oil reservoir

5.1. Open or closed system

Heat transfer systems can be designed as open or closed systems.

5.1.1. Open system design

Open systems are characterised by an expansion tank that is vented to the atmosphere.
This allows for oxygen entry and the possibility for oil oxidation.

5.1.2. Closed system design

Closed systems are those where the expansion tank is sealed from atmosphere. This
can be achieved with nitrogen blanketing, expansion bellows or a floating piston in the
expansion tank. Generally, the temperature of the expansion tank should be below
55°C (130°F). This essentially eliminates oil oxidation.

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 VENT
Legend:
T: Temperature Gauge
P: Pressure Gauge
F: Filter
EXPANSION PROCESS
TANK VESSEL
VENT

HEATER T

T
P
T

P
P
P
P
T F
CIRCULATING
PUMPS
Figure 4, Typical heat-transfer system

5.2. Heating unit

Typically the heating unit derives its energy from an electrical element, a combustion
furnace (gas or oil), or steam.

The heating unit is the most critical part of a heat transfer system because of its
possible effects on the heat-transfer oil:
• For combustion type heaters, the maximum tube wall temperature should not
exceed 360ºC (680ºF) and flames should not contact the tubes (also known as
direct flame impingement) in order to avoid thermal damage to the heat-transfer
oil.
• For immersed electrical heaters, the heat input rate should not exceed 2.6
Watts/cm2 (16 Watts/in2) of heater surface. However, depending on the flow rate
of the system and fluid used, these values can be reduced by one half. At rates
above these values, localized coking can occur. Note: These values apply only
to heat transfer systems due to their high flow rates. The maximum heat input
rate for standard lubrication applications (gearboxes, hydraulic systems, etc.) is 1
Watt/cm2 (6 Watt/in2) of heater surface due to these systems' much slower oil
flow rates.

To avoid hot spots, oil flow must be directed over the heating surfaces so that there are
no areas of stagnant oil. Stagnant oil will quickly become overheated and can lead to

14
deposits which insulate the surface thus interfering with heat transfer. These deposits
can create hot spots or lead to piping rupture.

It is critical to have a safety device that will shut off the burners in case of a pump
shutdown.

5.3. Pumps
The pump is the driving force circulating the oil through the system:
• It must have the capacity to circulate the oil at a rate that will provide the heat
required by the users, plus heat losses, with a reasonable temperature drop of
10 to 20°C across the users.
• The flow rate should maximize turbulence over the heater surfaces so as to
minimize thermal stress on the fluid and to promote efficient heat transfer.

Also:
• Pumps must be suitable for high-temperature fluid service.
• The pump should discharge to the heater.
• Pumps should be located at a level sufficiently below the expansion tank to
provide the necessary static pressure head required by the pump.
• The lubricating oil of the pump should be separate from the heat transfer oil.
• Rotary pumps are preferable to centrifugal pumps as the latter are more subject
to cavitation if the oil's vapour pressure rises excessively during service.

5.4. Filters
Heat transfer systems require excellent filtration because this is critical to fluid and
system longevity. Filters serve two main purposes in that they prevent suspended
foreign matter from damaging the pump and also prevent this material from being
deposited in other portions of the system.

Deposits will have many negative effects on the system:

• They will constrict passageways which will reduce turbulence and increase
thermal stress on the fluid.
• They will insulate heater surfaces causing hot spot in other areas; insulated heat
transfer surfaces will provide less heat to the user and negatively impact the
process.
• Debris build-up will accelerate the deposition of additional deposits.
• Deposits and soluble oxidative materials will act as catalysts and oxidize fresh oil
much more readily than if they were removed.

A coarse strainer should be located between the reservoir and the pump inlet to protect
the pump from coarse contaminants (fine filtration can cause pump cavitation due to
pressure drop).

A kidney loop filtration system capable of 10% to 15% flow and resistant to very high
operating temperatures should be installed on all heat transfer systems. Although

15
guidelines from manufacturers are not generally available, 10 micron filtration systems
appear to be effective.

5.5. Process vessel - user

The process vessel is the vessel in which the heat is delivered to the material being
heated. Copper and copper alloys should be avoided as these promote oil oxidation
and sludge formation.

5.6. Expansion tank

The expansion tank should be equipped with fittings so that an external filtration unit
can be easily connected to the tank in the event that a supplement to the existing
system filtration is required. Furthermore, the tank should be equipped with drains and
access points so that the tank interior surfaces can be easily cleaned.

5.6.1. Size - Thermal Expansion

The expansion tank is a necessary part of the system because, like all fluids, petroleum
oils expand when heated. The expansion varies with the temperature rise and the fluid
involved. Expansion can be considerable and the system must have the means to take
care of it.

This vessel also provides a hydrostatic pressure on the rest of the system. For this
reason, it is usually located at the least three meters higher than the rest of the circuit.

The degree to which a lubricant expands when heated is expressed by its thermal
expansion coefficient. This value should be provided in a fluid's data sheet.

The expansion of the fluid can be calculated from the equation:

Increase in volume = Coefficient of thermal expansion x Rise in temperature (°C) x Initial volume (L)

For example, in a system using Thermoil 32, with a coefficient of thermal expansion of
0.00080 (per °C), that has 5000 litres of piping, where the difference between average
ambient temperature and system operating temperature is 210°C, the calculation would
be:

Increase in volume = 0.00080 X 210°C X 5000 L

= 840 L

Therefore, in this example, the fluid in this system would expand by 840 L from ambient
to operating temperature. The expansion tank must be able to accommodate this
volume change.

The general rule is tank capacity should be twice the calculated expansion volume.
That is, the tank should be 25% full when the system is cold and approximately 75% full
when the oil is hot. Therefore an expansion tank of approximately 1600 that is 25% full
when the system is cold would be appropriate.

16
 5.6.2. Oxidation control
The surface of the heat transfer oil in the expansion tank is the principal part of the
system where oxygen may come in contact with the oil and possibly cause oxidation.
Therefore careful thought must be given to the design of the expansion tank to promote
the maximum service life of the heat-transfer oil:

• A vertical tank with a relatively large height to diameter ratio will minimize the
amount of oil exposed to air.
• The temperature of the oil in the tank should not be more than 54ºC (130°F), if it
is vented to the atmosphere, to reduce the rate of oxidation.
• To maintain cold oil in the expansion tank, the tank and connecting piping should
NOT be insulated.

If the oil temperature in the expansion tank cannot be kept below 54°C (130°F), an inert
gas, such as nitrogen, may be used to maintain a slight positive pressure in the
expansion tank. The tank should be outfitted with an oil level gauge, a thermometer, a
vent line from the top of the tank, a drain, an overflow line, and a filling connection.

17
6. Heat Transfer System Operation
SUMMARY OF HEAT TRANSFER SYSTEM OPERATION:

INITIAL FILLING:
9 Consider a system flush before commissioning (to eliminate contaminants and water)
9 Filling of the system should be done so that air is not introduced or, alternatively, is removed
during the process.

START-UP:
9 Temperature should be raised slowly while fluid is allowed to circulate at full flow.
9 Air and water must be allowed to leave the system.

REGULAR OPERATION:
9 To prevent hot spots developing, circulation pumps must always be in operation, with full
fluid flow passing through the heater before start-up.
9 To prevent stored heat from forming damaging hot spots, the heater must be shut off before
the pumps so that the oil can circulate and dissipate heat.
9 The system should be inspected regularly to ensure it is operating within design parameters
and to check for hot spots and leaks.

WATER CONTAMINATION:
9 Water in a heat transfer system can be an equipment and safety hazard. Water levels must be
kept to a minimum to prevent explosive reactions.
9 Low levels of water will manifest itself as pump pressure fluctuations (cavitation).

SYSTEM CLEANING:
9 Effective heat transfer system cleaning is very challenging if a system has been neglected. In
most cases, a detergent product is required to dissolve accumulated soft deposits. In the
case of very dirty systems, caustic cleaners (applied by specialised contractors) may be the
only means of removing hard deposits.

SYSTEM MAINTENANCE:
9 During system maintenance, fluid flow should be continued to prevent sediment dropout and
start up problems
9 Leaks or spills must be addressed immediately.

6.1. Initial Filling

A system flush is recommended prior to commissioning (see the section on Flushing
page 22).

Prior to filling a new system, all safety and control devices should be in working order.

The system should be pressure tested for leaks. In order to minimize problems with
water, water must NOT be used for system pressure testing.

It is best to purge all piping, equipment, and reservoirs with an inert gas prior to
charging the system with heat transfer fluid. Using inert gas that is heated can help
vaporize more of the water trapped within the system, making for a more thorough job.

18
If possible, the heat transfer fluid should be allowed to sit and warm up to at least room
temperature before filling the system as this will allow air bubbles, which may have been
entrained in the fluid during shipping, to rise out of the fluid.

Filling of the system should be done so that air is not introduced or, alternatively, is
removed during the process. Preferably, the system can be filled through a connection
at the lowest point in the system. Pumping the oil in at this point will force air ahead of it
and out of the vents, which must be open until the air is purged and the oil appears at
each one. Alternatively, a vacuum pump at the expansion tank can be used to remove
the air as the system is filled. This also helps to remove moisture.

All vents should be open during filling and closed as soon as the air is purged and fluid
appears.

In all cases, the fluid should be circulated through the system for up to 4 hours to
eliminate air pockets and to be certain that the fluid level is correct. This must be
completed with the heaters turned off. The expansion tank should be one-quarter full
when the system is cold.

6.2. Start-up
After the initial fill and period of cold oil circulation, the pump strainers should be
removed and cleaned, if necessary, and reinstalled. The condition of the filters should
also be examined.

The heater can then be started. The full heat output of the heater should be switched on
only after fully turbulent flow has been established within the heater or vaporizer tubes.

On initial and all subsequent start-ups from cold, the temperature should be raised
slowly [about 56°C (100°F) per hour]. This gives the system time to gradually expand
and drive off any moisture. Also, this avoids unusual stresses in the equipment and
prevents rapid vaporization of any trapped water which could lead to system overflow or
rupture. The system pump must be delivering full flow during this period to ensure that
the fluid is not in the heating unit longer than necessary which can cause thermal
cracking if a critical temperature level is reached.

Any water that is present during the heating-up period will expand. This may cause
"bumping" and force oil into the expansion tank. In severe cases, frothing may occur
and oil may overflow from the vents. Slowly raising the system temperature will
minimize problems with water as long as some of the water vapour can be released,
i.e., the expansion tank and vents may have to be opened so that any air and water
vapour can escape.

Base-line readings of steady-state values for thermometers and pressure gauges

should be taken for future reference.

19
 6.3. Regular Operation
A visual examination should be made at least once daily of the inside of the heater or
vaporizer combustion chamber using available observations ports, to check for any
small but visible heat transfer fluid leaks (which would be burning). In combustion
heaters, the appearance of the flame should be checked to ensure that it appears
normal and is not impinging directly on any heat transfer surfaces, particularly after any
change in load. Tube surfaces should be checked as much as possible for evidence of
overheating. Unusually coloured tubes may indicate coking or plugging. Infrared
scanners may also be used for a more precise examination.

The system should be operated within the temperature and pressure limits specified by
the supplier or manufacturer of the heat transfer fluid and by the manufacturer of the
equipment. If operation above design conditions is desired, the equipment
manufacturer should be contacted so that maximum safe operating conditions may be
established.

To prevent hot spots, circulating pumps should always be in operation, with fluid flowing
through the heater before it is started. The heater should always be turned off before
stopping the pump. The pump should operate for at least 30 minutes after the heat has
been shut off to the prevent hot spots than can damage the fluid.

The system must not be operated with any safety devices out of service.

After each fuel shutoff, the inside of the combustion chamber should be checked for
glowing tubes due to fouling and plugging, burning heat transfer fluid from a leak, and
fuel leaking past the safety shutoff valve(s).

If it is suspected that the material being heated is infiltrating into the heat transfer fluid
loop, the system should be shut down and the internal leakage point found as soon as
possible.

6.4. Water contamination in heat transfer fluids

Water in a heat transfer system can be a safety hazard and a threat to the equipment.
When water residing at a low point in a system reaches its boiling point, its volume
increases suddenly by over 1,000 times as it flashes to steam. The displaced fluid is
quickly forced into the expansion tank and out the vent. Hot fluid and steam spurting
out of a vent can cause serious injury and even fire. In some systems, the rapid
expansion can cause a rupture of system piping and seals.

6.4.1. Water detection

Small water infiltrations of less than 300 to 400 ppm show up as pump pressure
fluctuations (cavitation). Sometimes, the fluctuations are misinterpreted or ignored
because a system’s heater-outlet temperature operates well above water’s boiling point.
However, the fluid temperature is lowest at the pump suction, and that temperature
determines whether the water is liquid or gas at that point in the system. If the

20
fluctuations start suddenly while the system is heating up, there are low levels of water
in the fluid.

High levels of water are usually easily observed as free water visible at the bottom of a
decanted sample.

Care must be taken to monitor sudden changes in a system; whether it is pump

cavitation, increased expansion-tank volume, unusual sounds or increased pressures,
especially during start-up. All of these can indicate water in the system.

6.4.2. Water removal

If the system has significant free-liquid water, as much of this water as possible must be
drained from the system low points.

When most of the free water is removed, remaining water can be “steamed off” by
running the system at about 107°C (225°F) with all vents and the expansion tank warm-
up valve open. (Because the change in volume when water turns to steam is about
1,000 to 1, very little water is required to create a lot of steam.)

To ensure complete removal of water, the expansion-tank temperature must be

maintained above 100°C (212°F) to prevent vapour condensation, and nitrogen should
be added to the expansion tank headspace to sweep the water vapour from the tank as
it is generated.

Once the system is stable, a water check should be performed at all the low-point drains
in the expansion tank.

6.4.3. Best practises

It is impossible to keep a hot oil system 100 % free of moisture, but even minimal
precautions will help prevent water from being a major concern.

Do not use water to pressure test (hydro-test) a new system. It is better to use an inert
gas such as nitrogen if a system must be tested.

If a system component is being replaced, make sure the service personnel dry it
thoroughly before installation if it has been hydro-tested.

Product drums must be not stored outdoors where water can collect in the drumhead.
The expansion and contraction of the fluid with temperature changes can pull water in
through the bungs. If drums must be stored outdoors, they should be laid on their sides
with the bungs horizontal to the ground. After unsealing a drum, the fluid should be
discarded if there is rust on the seal itself or on the drumhead.

21
 6.5. Flushing
6.5.1. Commissioning
When a heat transfer system is commissioned it is advisable to perform a flush of the
system to ensure that any debris (sealing material, metal particles, etc) or cleaning
agents are removed prior to putting the system into operation.

It is recommended to perform the flush with the same product that will be used during
operation. Depending on a site's needs and comfort level, it may be possible to re-use
the flushing fluid to charge the system if the post-flush fluid analysis is satisfactory.

During a flush, the fluid should be circulated for a minimum of 24 hours. The condition
of the filters should be monitored during the flush and changed as required. At a
minimum, the filter should be changed when the final charge of fluid is made in the
system.

The filtration level chosen for a flush should be appropriate to the level used during
normal operation. For example, if a 10 micron filter will be used during regular
operation, one should work down through filtration levels during flushing from 100
micron to 25 to 10 micron.

6.5.2. Cleaning
Heat transfer system manufacturers do not tend to provide a great deal of
documentation regarding the cleaning of their systems. However, due to the current
trend to operate these systems at or above their design levels, the oil is under stress
and these systems require periodic cleaning.

Since it is impossible to completely drain all lines and low spots, flushing fluid will
remain in a system. Therefore, products such as heating oils and solvents should be
avoided for flushing purposes as the remains of these will evaporate during operation
and become a fire hazard. As well, chemicals or water-based cleaning agents will
contaminate the system. Steam can potentially rupture system piping.

The preferred product for flushing is mineral oil. If the system is suspected of being
very dirty, detergent product can be used, such as Exxon System Cleaner (ESC). ESC
is a detergent dispersant. It will release hydrocarbon materials and keep them
dispersed for filtration. ESC will remove some materials, but it will not be able to
dissolve harder carbonaceous materials effectively.

• It is recommended to add ESC at a 20% maximum concentration. Higher levels

may release too much of the sediment too quickly, overwhelming the system
filtration, perhaps blocking pipe work in the process.
• Good filtration is required for this product to be most effective. Using a high
detergent oil will release a substantial amount of contamination and a sufficient
number of filters must be on hand to accommodate this. The filter size chosen
for a flush should relate to the size used during operation; therefore one would

22
 work down from 100 micron to 25 to 10 micron during a flush. Starting with less
efficient elements will help remove the larger lumps and chunks first.
• The flushing medium should be circulated while hot, above 85°C (185°F), and
circulated for at least 48 hours and then drained while still hot. Flushing duration
and effectiveness can be reduced by raising system temperature. Of note, a 24
hour flush with system cleaner at 55°C (130°F) can be reduced to approximately
2 hours at 150 °C (300°F).
• Velocity of the flush is also important. Turbulent flow should be maintained.

Ideally, the system should have a clean-out door or trap so that sludge that is deposited
in the expansion tank and heating unit can be removed manually. After the flush is
complete, the condition of the flushing fluid should be examined, as well as the filters in
the system.

In cases where a heat transfer system has hard carbonaceous deposits that cannot be
removed using a detergent oil flush, sodium caustic flushes are sometimes used. This
is a very reactive material which is very difficult to handle and difficult to use effectively.
Furthermore, the flush has to be followed with high-pressure water cleaning which must
be removed before the system is put back into operation. This type of flushing should
only be carried out by a qualified firm specializing in this type of work.

6.6. System Maintenance

During shutdowns, fluid flow in the system should be continued. The potential dangers
of no flow are sediment dropout and deposit formation, which will be followed by flow
problems on subsequent start up. If the heat transfer system is being serviced, the area
being worked on should be isolated with circulation continued everywhere else. Also,
keeping the system warm - 80°C (175°F) - is advisable as it helps to keep contaminants
in solution so that they can reach the filters and not deposit in the system. Filtration of
the circulating fluid should also continue. If necessary, a portable unit should be rented
during the downtime.

Depending on the condition of a system, a site may want to flush the boiler loop during
each and every shutdown.

Any and all system leaks that are discovered should be corrected promptly, regardless
of how small they may be. Corrections should be of a permanent nature, such as
repacking valve stems and replacing leaky gaskets. Any fluid spilled from a leak or from
safety valve operation should be cleaned up immediately if it is (or could be) in contact
with a hot or warm surface. Other spills should be cleaned up at the first available
opportunity.

Any pipe or equipment insulation that is discovered to be oil-soaked should be promptly

removed and replaced with clean, oil-free insulation, and the cause of the leak
corrected.

23
7. Safety
SUMMARY OF HEAT TRANSFER SYSTEM SAFETY:

9 Operators must be trained in safe heat transfer system operation.

9 In order for the fluid to ignite many conditions must be satisfied simultaneously:
• the fluid must reach its flash point,
• the system must suffer a leak where vapours can escape, and
• there must be a source of ignition close to the leak.

9 In order to minimize the potential for fire:

• Optimal heat transfer fluid condition must be maintained.
• Heat transfer systems should be located in areas with adequate ventilation.
• Heat transfer systems must be maintained to prevent leaks and failures.
• Soiled insulation should be replaced as soon as possible.
• Systems should be thoroughly inspected during shutdowns for sign of leaks.
• Flow must be maintained across heaters so that fluid overheating is minimized.

7.1. Operator Training

All operators involved with heat transfer systems should be provided with a formal
training program detailing the proper operation of the heat transfer system. This should
include:
• Emergency procedures to be taken in the event of process control upsets and
emergency conditions.
• Hazards relating to incorrect heat transfer system operation and leakage.
• Recognition of upset conditions that could lead to dangerous situations.
• Refresher training should be given to all operators at least annually.

Table 1 lists the time required to develop a third degree burn at different water
temperatures. These temperatures are well below the operating temperatures of heat
transfer oils and can be used to highlight the caution that is required when working on
and around these systems.

Table 1, Water temperature and time required to develop a third degree burn
Water temperature Time required for a third
°C (°F) degree burn
68 (155) 1 second
64 (147) 2 seconds
60 (140) 5 seconds
56 (133) 15 seconds
52 (126) 1 minute
51 (124) 3 minutes
48 (118) 5 minutes

24
Heat transfer systems must be designed and operated to ensure that the oil and the
material being heated do not commingle as, depending on the material, chemical and
thermal reactions can take place.

7.2. Fire Prevention

From a safety perspective, flash point is the most commonly used test to determine the
suitability for continued use of a heat transfer oil. However, these fluids typically
operate at temperatures considerably above their flash point. Therefore, although these
tests measure the ease with which a fluid will ignite, this information must be interpreted
in the context of the respective heat transfer system.

In order for the fluid to ignite, many conditions must be satisfied simultaneously:
• the fluid must reach its flash point,
• the system must suffer a leak where vapours can escape, and
• there must be a source of ignition close enough to the leak to ensure a
concentration of vapour that is sufficiently high to ignite.

Under normal circumstances, leaking fluid will cool very quickly to below its flash point
when exposed to air; this is the main reason why fires originating in heat transfer
systems are a relatively rare occurrence.

In order to minimize the potential for fire in heat transfer systems, a number of steps
should be taken and are listed below1. These steps are in addition to maintaining the
heat transfer fluid and protecting it against oxidation and thermal cracking, as described
throughout this document.

7.2.1. General considerations

Heat transfer systems should be located in areas with adequate ventilation to prevent
the build-up of vapour. Systems that have the potential to spray flammable fluid (such
as hydraulic systems) should be located well away from heaters. Catch drums that are
used to collect material discharged from the expansion tank (water or light ends) should
be drained regularly since these materials can create vapour if hot fluid is discharged
onto them.

7.2.2. Insulation
The most common type of heat transfer system fire is one that occurs when the fluid
leaks onto insulation material that allows the fluid to disperse. This permits the
concentration of vapours that can ignite with a sudden increase in available oxygen or a
change in temperature. For this reason, it is recommended to use close-cell insulation
material to contain fluid in the event of a leak. Open-cell insulation, that allows the fluid
to disperse, should only be used where the possibility of leakage is very small. Soiled
insulation should be replaced as soon as possible.

1
Oetinger, J., "Prevent Fires in Thermal Fluid"," Chem. Eng. Progress, January 2002.

25
 7.2.3. Loss of flow
If an equipment failure stops or reduces the flow of the heat transfer fluid across the
heater, the temperature of the stagnant oil could rise rapidly above its boiling point and
its auto-ignition temperature. The vapour that is then created can violently discharge
fluid into a catch tank from the expansion tank. Therefore, it is critical that appropriate
flow meters be installed on heat transfer systems and that pumps are sized to provide
sufficient flow rate under all operating conditions. Furthermore, low flow shutdowns
should be included in system controls.

7.2.4. Major leaks

A major mechanical failure of a heat transfer system could allow a significant quantity of
fluid to leak onto an ignition source. Sources of ignition could be malfunctioning
equipment such as failing bearings, seizing equipment or sparks created by rotating
components. Effective maintenance of heat transfer systems is essential in reducing
potential sources of ignition.

7.2.5. Cracked heater tubes

If a crack is created inside a heater tube, leaking fluid will burn off immediately as it
contacts the heating element. This burning liquid can normally be seen in heater sight
ports. If a crack allows a large volume of fluid to accumulate inside a heater, for
example during a shutdown, the start-up of the heater would ignite this accumulated
fluid and would likely destroy the heater. The condition of heaters must be reviewed
during all shutdowns.

26
8. Oil Life - Used Oil Analysis
SUMMARY OF USED OlL ANALYSIS:

9 Regular used oil sampling should begin as soon as a system is put in service and should
continue throughout the life of the system.
9 A disciplined fluid monitoring program can alert users to the early warning signs of problems
if the fluid is oxidized, thermally degraded or contaminated and can allow users to take action
before expensive shutdown maintenance is required.

SAMPLING:
9 Sampling safety is a primary concern due to elevated system temperatures.
9 Sampling procedures must be consistent and must ensure clean and representative samples.
9 Systems should be equipped with a sampling device for the hot circulating loop

ANALYSlS:
9 At a minimum, a heat transfer fluid should be analyzed every six months and the monitoring
program should involve regular analysis of: Kinematic Viscosity (KV), Total Acid Number
(TAN), Water %, Sediment, Flash Point, and Metals.
9 An optional test is Simulated Distillation by Gas Chromatography (GCD).

There is no simple way to judge the suitability of an oil for continued service in a heat
transfer system. The decision must be made based on the accumulated results of
regular used oil analysis. Parameters from fresh oil and results for a series of samples
for the oil in service, provides the basis for deciding if the oil is suitable for continued
service or not.

A disciplined fluid monitoring program can alert users to the early warning signs of
problems if the fluid is oxidized, thermally degraded or contaminated. In the case of
heat transfer fluids, fluid analysis can characterize the heat-transfer performance of the
fluid, but also provides important information on the suitability for continued use of the
fluid from a safety perspective.

With enough data points, the rate of degradation can be determined, and then
extrapolated to project remaining fluid life. This information will allow users to implement
early corrective actions before the situation escalates into a problem that causes an
emergency shutdown. Also, the accumulated data can be reviewed to determine if the
problem is fluid or system related.

Most often, heat transfer system fluids are not analyzed until a problem occurs.
Generally, at this point, the results indicate that the fluid has degraded extensively and
the by-products have polymerized (combined) and deposited throughout the system.

If a fluid is changed out before its condemning limits are exceeded, the system
only requires draining and fluid replacement, without the need for flushing or
system cleaning. Continued use of an extensively degraded fluid will eventually
lead to hard carbonaceous deposits, necessitating complex and expensive
system cleaning.

27
 8.1. Sampling procedures
Using a proper and safe sample point and sampling procedure is critical for a heat
transfer system due to the elevated temperatures of the system. Also any exposure to
air can negatively affect water content, flash and other results.

8.1.1. Consistency
To get accurate results and to effectively monitor trends, sampling procedures must be
consistent from one sample to the next. Samples should be taken from the same
sampling point each time, and also at a consistent time in the machines’ maintenance or
operation.

8.1.2. Cleanliness
Cleanliness is essential when sampling equipment:
• Only new sample bottles should be used and they should be kept closed until
samples are taken.
• Dirt from around sampling points or drain plugs must be removed.
• Ideally the sampling tube should be flushed with the oil being sampled by an
amount equal to eight times the tube contents before drawing the sample.
• Degreasing agents should not be used for cleaning sampling equipment as
traces of these materials can seriously affect the analysis.

8.1.3. Sample Location

Ideally, in a heat transfer system, two samples should be taken:
• one from the flowing system, and
• one from the expansion tank.

These two samples are preferred since sludge may not be present in the tank or at the
point of sampling. If the sample is not taken from the hot circulating loop, it will not be
representative of the system fluid, and the results will be less significant. Also, in
certain systems, the nature of the oil in the flowing system and the expansion tank are
quite different. Sampling from the drain plug is not recommended due to the difficulty in
obtaining a representative sample. However, if this is unavoidable, at least 4L should
be drained prior to taking a sample.

8.1.4. Sampling devices

Systems should be equipped with proper connections and sampling devices to facilitate
direct fluid sampling from the hot circulating loop. Great care is necessary due to the
elevated oil temperatures.

Figure 5, illustrates an example of a safe sample model for sampling from the hot
circulating loop. In this case, valves are normally closed until a sample is required and
valves are opened well in advance to help flush the lines before taking a sample. The
flow is then closed to the sample loop and the oil is allowed to cool in the loop until it is
below 65°C (150°F). The sample is drawn using a tight connection to avoid introduction
of air into the sample.

28
 Figure 5, Sample System Model

The sample container should be made of metal so that there

is no risk of it melting. Ideally, it should also connect to the
sample port with a tight connection so that no light
components in the sample are lost. However, if these are
not available, steel fuel sample containers are widely
available and are an effective secondary option, see Figure
6 . These containers must be closed quickly and tightly after
taking a sample in order to minimize the loss of light ends. Figure 6, Type 1 Safety Can

Appropriate personal protective equipment is critical (i.e. safety glasses, gloves, fire
extinguisher, etc.).

8.1.5. Recording sampling data

Sample details should be recorded as completely and accurately as possible. This is
critical to the meaningful interpretation of the analysis results and includes:
• Equipment ID • Make-up Oil added
• Equipment hours • Sample location
• Oil hrs • System temperatures (operating and
• Oil-in-Use Name expansion tank)
• Sample Date • System status (start-up, active or re-start)

8.1.6. Frequency
Every time a new system is started, or an oil change-out is performed, an initial sample
of new oil should be analyzed to provide a baseline for future samples. Following this,
sampling and analysis should be done every quarter. This can be reduced to twice per
year provided the results indicate that the oil is suitable for continued service. Any time
the bulk oil temperature is exceeded, a sample should be taken for analysis.

8.1.7. Sample Volume

In order to ensure sufficient sample volume to complete all necessary testing, at least 1
L of fluid should be drawn from each sample point.

29
 8.2. Typical Analysis
A complete heat transfer fluid monitoring program should involve regular analysis of the
following parameters:
• Kinematic Viscosity (KV) at 40ºC and 100ºC
• Total Acid Number (TAN)
• Water %
• Sediment
• Metals
• Flash Point (Open-cup and, if indicated, closed-cup)
• Simulated Distillation (GCD) (optional)

Daily monitoring of the system's operating parameters, including the inlet and outlet
temperatures and pressures at the heat source and users, can also provide a means for
early detection of potential system problems.

8.3. Kinematic Viscosity (KV)

Viscosity is a measure of a fluid's resistance to flow, or in laymen's terms, a measure of
a fluid's thickness. Viscosity is often the first consideration in the selection of a
lubricating oil because the primary purpose of a lubricant is to reduce friction and
minimize wear by separating surfaces with an oil film. However, in the case of heat
transfer fluids, the importance of viscosity relates to its heat transfer efficiency and the
ease of flow of the oil through the system in order to minimize pumping losses.
Furthermore, changes in a heat transfer oil viscosity can signal oil degradation.

8.3.1. KV Test Details

The most common method of expressing an oil's viscosity is its kinematic viscosity,
which is measured by the time required for a fixed volume of oil to flow through a
capillary tube as described in ASTM test method D445. The test is usually run at fixed
temperatures (40°C and 100°C) and the results are reported in centistokes (cSt), with
higher values indicating a thicker oil. The ISO grade of an oil relates to its viscosity,
measured in cSt, at 40°C.

8.3.2. KV Test Results

Any large increase in viscosity accompanied by an increase in TAN (see below) usually
indicates that the oil is suffering the effects of oxidation. For further details on oxidation,
see section 4.2 Oxidation, page 12.

A decrease in viscosity can indicate contamination with a lighter product or thermal

cracking. A decrease in viscosity with no change in TAN can be used as an indicator of
thermal degradation since low boilers will tend to reduce viscosity.

Most laboratories will highlight viscosity as a concern when it changes 10% from the
original ISO grade.

30
 8.4. Total Acid Number (TAN)
Depending on its additive content, refining procedure, or deterioration in service, a
petroleum oil may exhibit certain acid characteristics. The acidic content of an oil
sample is usually expressed in terms of its total acid number (TAN).

As described in section 4.2, Oxidation, on page 12, oils that are exposed to oxygen will
oxidize. The major by-products of oxidation are organic acids, which will increase the
acidic content of the oil and therefore increase its measured TAN. These acids will, in
turn, tend to accelerate the molecular breakdown of the heat transfer fluid; and, will tend
to form insoluble sludge that accelerate mechanical deterioration of seals, valves,
pumps, etc.

It must be noted, however, that the TAN of a used oil is meaningless unless it is
compared with the TAN number of the new oil. When interpreting TAN test results, it is
the amount and rate of change that is important to understand used oil quality.

8.4.1. TAN Test Details

As described in ASTM test method D664, the TAN of an oil is the weight in milligrams of
potassium hydroxide required to neutralize one gram of the oil.

8.4.2. TAN Test Results

A rise in TAN is generally indicative of increasing oxidation since organic acids are
formed as a result of oxidation. Acid number increase usually is associated with open
vent expansion tank operation. Process material containing oxidizing agents can
sometimes also contribute strong or weak acids.

Most heat transfer fluids have an initial total acid number less than 0.50. The maximum
value in used fluid should not exceed 3.0.

The oxidation process generally starts slowly and then as the acid content of the oil
increases, these oxidation by-products accelerate the reaction. Therefore, an initial
slow increase in TAN number is expected; however, once the results begin to increase
rapidly, the oil is nearing the end of its service life.

8.5. Water
Water in heat transfer systems is very problematic as water can be a safety hazard and
a threat to the equipment. Concerns and corrective actions related to water
contamination are described in section 6.4, Water contamination in heat transfer fluids,
on page 20.

Water is also a catalyst to oil oxidation and rust formation; therefore high water content
must be addressed through corrective action.

31
 8.5.1. Water Test Details
High levels of water are usually easily observed as free water visible at the bottom of a
decanted sample of fluid.

The water content of oil is typically measured by Karl Fischer Titration, as defined by
ASTM D1744. This test detects the concentration of water in the fluid by using a
reagent that reacts with the water in the oil and depolarizes an electrode. The resulting
voltage change is used to determine the endpoint of the titration and thus calculate the
concentration of the water in the oil sample.

8.5.2. Water Test Results

The moisture content of an oil is a primary indicator of the integrity of a water/fluid
interface, such as in water-cooled heat exchangers or reactor jackets in which water is a
component of the product being processed. Although some moisture from humid air
may be drawn into the fluid through improperly blanketed expansion tanks or during the
cooling phase of sample collection, moisture levels in excess of 500 ppm (0.05%) or the
presence of free water in a sample generally indicate a failure at a water/fluid interface.

Initially, water/fluid interface failures are usually not dramatic. Generally, the leak is of
the "pinhole" variety, and system pressures are not noticeably affected at the onset. If
high water content is detected sample frequency should be increased to confirm and
monitor the situation, and plans should be made to examine or repair the appropriate
heat exchange surface at the next scheduled shutdown. Should moisture levels in
subsequent samples increase, or the system begin to pressurize excessively, more
immediate action may be required.

Water content above 250ppm should be investigated; water content at 1000ppm or

greater is cause for corrosion, and potential safety concerns.

8.6. Sediment
System cleanliness is an important consideration for any industrial system. This is
particularly true for heat transfer systems where the circulating fluid can:
• act as carrier for damaging abrasive particles, or
• can degrade and create insoluble particles that deposit in the system thereby
reducing its heat transfer efficiency, plug system piping, or acts as catalysts for
further fluid degradation.

As with any oil circulating system, there is an optimum cleanliness level that will provide
maximum system and oil life by protecting internal components from abrasive wear
particles and fluid degradation by-products before they are distributed in the system.

The cleanliness of the system and the appropriateness of its filtration system can be
assessed by measuring the sediment content of the oil.

32
 8.6.1. Sediment Test Details
The presence and amount of sediment in an oil can be measured using test procedures
based ASTM D2273. This method determines the amount of suspended solids in an oil,
which may include metallic debris, dirt and other foreign materials.

This test involves a dilution of equal parts of sample and solvent in a test tube. The
sample is mixed and then placed in a centrifuge. The sample is then spun, which forces
insoluble sediment to the bottom of the tube. The resulting sediment volume is
measured and expressed as a volume percent.

8.6.2. Sediment Test Results

It is quite common to measure high sediment content in new systems after start-up, due
to construction debris, or in older systems that have never been filtered.

High sediment levels can also be a result of thermal cracking or oxidation because the
by-products of these processes can include hard carbonaceous deposits that can be
captured in this test.

Sediment levels above 1.5% should be treated with concern as these higher than
normal sediment levels can begin to reduce pipe diameters and system flow. The
filtration on these systems should be evaluated and, if necessary, portable filtration units
should be used until the oil is cleaned.

Sediment levels above 2% are considered critical and action must be taken as soon as
possible to bring the oil back to acceptable levels.

8.7. Metals (ICPES)

Contamination in a heat transfer system can come from outside sources, fluid
degradation or can also be the result of system component wear. Some of these
contaminants will contain metal which can be measured using spectrometric analysis
(measuring emissions from a sample).

The metals identified in spectrometric analysis will reflect both the additive metal
content of the oil, metals coming from outside contaminants or the metals derived from
wear of specific parts of the equipment in which the oil has been used. Regardless of
their source, allowing contaminants to circulate through the system may accelerate
wear of components and in some cases accelerate fluid degradation. Typically, metals
analysis permits the early identification of mechanical failures which allows the
opportunity to correct the problems before they lead to an emergency shutdown.

While spectrometric analysis can give very valuable information on the condition of the
oil and equipment, considerable experience and knowledge of the equipment, the type
of service, the characteristics of the fresh oil as well as the characteristics of the
analysis method are required for reliable interpretation.

33
 8.7.1. Metals Test Details
ICPES (Inductively Coupled Plasma Emission Spectrometry) uses ICP (inductively
coupled plasma) to produce excited atoms that will emit electromagnetic radiation. The
radiation will be emitted at wavelengths characteristic of particular elements and the
intensity of this emission is proportional to the concentration of the elements within the
sample. However, these methods only detect submicroscopic metal particles (typically
less than about 10 microns). It is important to note that some types of equipment wear
or failure lead to larger metal particles which would not be detected in a routine used oil
analysis.

8.7.2. Metals Test Results

The interpretation of these results is very application specific as the results will vary
based on the metallurgy of the system in question:
• The metals that are of most concern are those associated with pump or oil
system components. As mentioned earlier, new systems put into service may
exhibit high metal content due to construction debris; however, in the case of a
system with adequate filtration, this should decrease quickly.
• Metals that are not associated with system components or oil additives are
typically the result of outside contaminants and may indicate a leak in the
system, infiltration of process materials into the heat transfer system or the
presence of another lubricant.

Generally, a metal step change over 10 ppm should be investigated; an increase of 20

ppm would be cause for concern and the source should be identified as soon as
possible to put corrective measures in place.

8.8. Flash point

As defined earlier, the flash point of an oil is the temperature at which the oil releases
enough vapour at its surface to ignite when an open flame is applied. At the flashpoint
of a liquid, the release of vapour is not sufficiently rapid to sustain combustion and the
flame will quickly extinguish. However, if heating is continued, a temperature will be
reached at which vapours are released rapidly enough to support combustion. This
temperature is called the fire point.

Other than through contamination with a more volatile fluid, the only way to reduce the
flash point (and fire point) of a fluid in a heat transfer system is through high
temperature thermal cracking of the hydrocarbon chains. As described in section 4.1,
Thermal cracking, this will create shorter hydrocarbon chains (low boilers) which results
in lighter flash materials. Other compounds resulting from thermal degradation will
combine into higher molecular weight and higher flash point molecules (high boilers).
These high and low boilers typically have lower heat transfer efficiency and thermal
stability than the original heat transfer fluid molecules. Furthermore, the low boilers that
cause the reduction in flash point are also a concern from a safety perspective in the
event of a leak from the system.

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Although there is much focus on the flash point of heat transfer oils, it is important to
remember that flash point is only one of several important tests to determine an oil's
suitability for continued service.

8.8.1. Flashpoint Test Details

Flashpoint can be measured by two methods: the the Cleveland Open Cup (COC)
Method (ASTM D92) or the Pensky-Marten Closed Cup (PMCC) Test (ASTM D93). In
both methods, a sample of oil is heated at a rate of ~10°F per minute. In the COC
method, the oil is placed in an open cup and at every 5°F rise in temperature a small
flame is passed over it. In the PMCC test the oil is placed in a closed cup and the cup
is opened momentarily and a flame is applied every 2°F up to 220° F and every 5°F
thereafter. When a momentary flash occurs the temperature reading is the flash point.

Fire point testing is essentially an extension of the COC Method. However, the
temperature is increased until combustion can be maintained for at least 5 seconds.
This temperature is the fire point.

8.8.2. Flashpoint Test Results

Open-cup Flash point by open-cup is typically the first test used to characterize the
thermal breakdown of a heat transfer fluid. There are a number of other tests that can
also be used to measure thermal degradation; however, flash point by open-cup is the
simplest method and can be used to determine if more in-depth testing is required.

If the flash by open-cup has not decreased significantly, then thermal degradation is not
significant from a performance or safety perspective. If flash by open-cup does show
significant flash reduction, then further analysis by other methods is warranted. It is
important to note that flashpoint only indicates that there are low boilers in a sample, not
the proportion of these components.

Flash test results, particularly by open-cup methods, are strongly impacted by sample
collection techniques: it is difficult to take a sample and capture a representative amount
of light ends. This could manifest itself as varying flash results from samples taken at
the same time. In the same way, sample handling has a large impact on test results.
For this reason, it has been acknowledged by the ASTM that lab to lab and sample to
sample variability is large, up to +/- 19°C. However, if care is taken to follow sound
sample collection techniques, the results would be adequate for the directional purpose
of this test.

The flash points of Imperial Oil's heat transfer fluids are available in the attached
product data sheet. Typically, a reduction in approximately 50°C in the flash point
measured by open-cup is cause for concern and further investigation.

Heat transfer fluids are commonly used at temperatures above their flash points. In
open systems, this is acceptable as long as the flash of the fluid is above the
temperature of the fluid in the expansion tank because this is the location in the system
that vapour collect in the system and could potentially escape.

35
Closed-cup The flash point, as measured by the closed-cup method is more sensitive
to the presence of low boilers (also called light ends) and can be used as a follow-up to
open-cup testing when open-cup flash test results begin to approach reportable levels.
Since the closed-cup method concentrates the light ends that evaporate from the
sample during the test, the flash point by closed-cup can be significantly lower than by
open-cup; 100°C differences are not uncommon.

Flash point by closed-cup should be 14ºC (25ºF) above the temperature of the oil at the
point of exposure to air, i.e. the expansion tank. Values lower than this are generally
considered critical. As open-cup and closed-cup flash results begin to decrease to their
reportable limits, analyzing the oil by GCD can shed additional light on the degree of
deterioration of the oil.

Fire point The fire point of a used oil is not generally used as condemning test for heat
transfer fluids because condemning limits for flash point are reached first.

8.9. Simulated Distillation by Gas Chromatography (GCD)

The Simulated Distillation by Gas Chromatography (GCD) test has not historically been
a routine heat transfer oil test. However, this test can be very informative from a heat
transfer performance and remaining life perspective because it can quantify the degree
of thermal degradation of a sample and the deterioration of its heat transfer
performance.

GCD is run as a follow-up to closed-cup flash where the flash results were approaching
reportable limits. GCD offers additional information to flash because it examines the
relative proportions of the entire range of molecules in the sample, whereas the flash
point test is only concerned with presence of lighter materials and not their proportions.

As explained previously, high and low boilers are formed when heat transfer fluids are
heated to a high temperature and molecular bonds begin to break or thermally degrade.
The low boilers have a lower molecular weight and typically a lower boiling point than
the original fluid. Other compounds resulting from thermal degradation will polymerize
(combine) into higher molecular weight and higher boiling point molecules: These are
referred to as high boilers.

Fresh oil has a boiling range because it is not a completely uniform product; there is
some variety in the sizes of molecules that make up the finished lubricant (as opposed
to water which has a distinct boiling point because it is relatively pure). As an oil
thermally degrades, and the proportions of different size molecules in the fluids
changes, the amount of product that boils off at different temperature changes as well.

8.9.1. GCD Test Details

GCD, as per ASTM D2887, defines the initial, intermediate and final boiling points of the
product being tested. This information can be plotted graphically, see Figure 7, to show
a distillation curve, i.e. the proportion of the sample that boils off at different

36
temperatures. When plotted against the distillation curve for fresh product, the
difference between the curves can quantify the change in the amount of lighter and
heavier material in the oil. The increases in the proportion of high and low boilers in a
heat transfer fluid are proportional to its thermal degradation.

It is important to note that the creation of light (and heavier) molecules through thermal
cracking will alter the shape of the entire curve, not just the initial part of the curve
because the creation of new molecules reduces the amount of the old molecules.

Figure 7, Typical GCD graphical analysis

8.9.2. GCD Test Results

There are no strict condemning limits when interpreting GCD results. Experience must
be used to determine what level of fluid degradation will have significant performance
impact on a heat transfer system. Generally a significant increase in the 5% off boiling
temperature, coupled with a change in the 10% off boiling temperature calls for
replacement of the fluid to maintain adequate heat transfer performance.

In the case of a dramatic increase in high or low boiler levels from the previous sample,
and with the fluid still operating within its maximum bulk operating temperatures, either
outside contamination, heater malfunction or decreased fluid flow rate may be assumed
to be the cause. In such a case, increased sampling is warranted and the process
pump flow rate and heater should be checked and examination of the heater tube wall
scheduled for the next shutdown.

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9. Troubleshooting Heat Transfer Systems
9.1. The vicious circle of heat transfer fluid degradation
Oil in a heat transfer system is exposed to extreme conditions. Depending on the
design of a system and the production pressures that are put on it, the oil can begin to
deteriorate through oxidation and thermal cracking. The deposits caused by these
processes have an insulating effect on heat exchange surfaces which generally requires
an increase in heater output to maintain production levels. This is a vicious cycle that
ultimately significantly reduces fluid life.
Heat transfer fluid is exposed to
extreme conditions:
• High temperatures
• Oxygen sources
• Contamination

Increase in temperatures is Oil begins to oxidize/crack:

required to maintain production • Viscosity increases
levels • Flash point increases
• By-products formed.

Deposits form on metal surfaces Contaminants accelerate oxidation

acting as insulators Oxidation accelerates oxidation

As in all industrial applications, once the heat transfer fluid no longer meets minimum
performance criteria this can have negative impacts on the process such as:
• Increase in system operating temperatures to maintain production
• Production issues
– Unable to maintain production rates
– Unable to meet heating requirements
• Increase in maintenance issues and costs
– Pump seal leaks
– Pump failures
– Control valve sticking
– Heat exchanger issues
• Quality issues
– Improperly cured product
– Raw materials or final product not meeting moisture requirements
• Excessive Expansion Tank Temperatures

It is important to identify the root causes of heat transfer fluid degradation so that the
vicious cycle can be broken.

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 9.2. Identifying root causes
Most problems that occur in heat transfer systems can be avoided by adhering to proper
design, operating and maintenance practices.

To effectively troubleshoot poorly performing heat transfer systems, follow these steps:

• Clearly define the problem based on observations and accumulated information.

• Review available historical system operation data and fluid condition analyses.
• List potential root causes and consider each.
• Identify the root cause based on the accumulated information.
• Execute corrective action.

Once the problem is corrected, the necessary changes in system design or operating
procedures should be documented and implemented to prevent a reoccurrence.

Troubleshooting is easier when the system's operating parameters and the fluid's
condition are monitored and analyzed routinely. The following should be available to
facilitate troubleshooting:

• Sufficient and properly located temperature and pressure gauges to monitor the fluid
at the inlet and outlet of each heat-user and the heat source.
• Up-to-date process and instrument drawing of the system as well as original
equipment specification sheets and fabrication drawings.
• System operating data from the period prior to and during the problem. This can be
compared with normal and historical data.
• Fluid analysis during the problem as well as historical fluid analysis data.
• Documentation of previous system problems.

9.3. Common symptoms and causes

If the following conditions develop, it is important to evaluate the possible cause and
implement corrective action.

9.3.1. Insufficient heat at user

If users on the system are unable to get the required amount of heat, possible causes
may be:

Fouled Heat Transfer Surfaces. Fouled heat transfer surfaces at the user are caused
by deposits of resinous carbonaceous material. This can develop if the fluid is thermally
cracked to form high boilers, see section 4.1 "Thermal cracking", page 9. Another
possible cause is fluid oxidation that leads to the products of oxidation polymerizing and
depositing on the heat exchange surface.

Fluid analysis can quickly identify if the fluid has been oxidized or thermally degraded.
Refer to section 8, Oil Life - Used Oil Analysis, page 27.

39
Historical operating conditions can be used as a cross-check to confirm fouling. If fluid
flow to the user is constant but the differential temperature across the user is reduced,
this indicates that the transfer surface is fouled.

Low Fluid Flow. Low fluid flow, due to partially plugged lines or filters as well as pump-
related problems, can also lead to insufficient heat at the user. Checking the pressure
differential across the pertinent piping or equipment sections will identify any blockages.

Low Fluid Temperature from the Heat Source. Low fluid temperature from the heat
source often is caused by progressive fouling of the tubes or the heat source's electrical
element. Other possible causes are reduced gas firing/watt setting or reduced fluid
residence time in the heat source.

Increased Viscosity. Increased fluid viscosity caused by the continued use of an

oxidized fluid can result in insufficient heat to the user. An excessive build-up of the
products of oxidation causes the fluid to thicken, and the higher viscosity fluid is less
efficient at transferring heat. Inadvertently contaminating system fluid with a higher
viscosity material also will increase its viscosity.

9.3.2. High Fluid Losses/Make-Up Rate

If the system constantly requires fluid additions, possible causes are:

Vapour Leaks from System. Heat transfer fluids that exhibit high vapour pressure
(chemical aromatics, for example) tend to leak from connections and fittings. If the
system's operating pressure is not set above the fluid's vapour pressure, fluid vapours
will vent continuously from the expansion tank, requiring frequent top-ups to maintain
fluid levels. Low vapour pressure fluids are preferred for liquid-phase systems because
they can be operated with essentially no pressure and minimum venting of vapours.

Leaks from Fittings and Connections. At the system operating temperature, metal
fittings and connections can expand, causing leaks. Another common cause of leaks is
using a seal material that is incompatible with the system fluid. To prevent leaks,
flanges and connections should be tightened while the system is at operating
temperature. If a system is frequently shut down and restarted, it is more likely to leak.
If the seals are incompatible with the fluid or (in the case of mechanical seals) if there is
insufficient cooling/flushing, leaks will occur frequently.

Thermal Degradation and Venting of Lighter Components. If the fluid being used is
not thermally suited for the application, it will thermally degrade. The low boilers
produced will be vented via the expansion tank. This problem is compounded if the

40
expansion tank is operated at elevated temperatures. This can also be an indicator that
the watt density of the heater is incorrect or malfunctioning.

There is a practise in industry known as "boiling off" whereby heat transfer systems
(and expansion tanks) are run at elevated temperatures in an attempt to boil off the
undesirable lighter components that have been created through thermal cracking.
Imperial Oil does not support this extremely hazardous practise as it concentrates
flammable vapours. If the system were to suffer a leak during the procedure these
vapours could ignite if a source of ignition were present.

High Fluid Level in Expansion Tank. If the fluid level in the expansion tank is too high,
some fluid droplets will become entrained with the vapours being vented. The
expansion tank's operating pressure should be higher than the fluid's vapour pressure
to minimize venting of fluid vapours.

9.3.3. Frequent filter plugging

Filter plugging reduces fluid flow and should be corrected. Possible causes are:

Polymerization. Frequent filter plugging indicates fluid polymerization and the build-up
of resinous sludge. Most often, this occurs when a fluid has been used well beyond its
condemning limits and has been extensively oxidized.

Fouling After Cleaning. Frequent filter plugging also can occur after an extensively
fouled or coked system has been cleaned and new fluid added. Residual solid particles
or sludge tend to accumulate on the filters during the initial operating period.

Increased Pressure Drop in the System. This can be caused by a restriction in the
piping network, filter plugging or increased system fluid viscosity. If not addressed, it
will lead to further problems.

9.3.4. Pump-related problems

Centrifugal pumps equipped with mechanical seals, water cooling on the bearings and a
seal flush system typically are used for fluid circulation in heat transfer systems.
Possible problems include:

Cavitation/Vapour Locking. Cavitation will occur if the system pressure falls below the
vapour pressure of the fluid being pumped, causing the fluid to vaporize and form
pockets of vapour. Pockets of water that periodically come in contact with hot fluid also
will create excessive system vapour.

41
Systems designed with inadequate venting capabilities allow pockets of vapours and
light ends to accumulate in the system, leading to cavitation and equipment damage.

Leaks. Frequent leaks from a pump with a mechanical seal indicates inadequate
cooling at the seal face. If the seal face temperature becomes excessively high, the
fluid in contact with the seal face will thermally crack and leave a hard carbon deposit.
The abrasive coke build-up will cause wear and eventually lead to fluid leaks. A
constant flow of low-pressure steam at the seal face can prevent this problem.

9.3.5. Noise in Pipes

Water. Most likely, noisy pipes are caused by water in the system. This can be caused
by water used in cleaning that is not removed during start-up. Water can be removed
by carefully circulating the hot system fluid through the expansion tank and allowing the
water vapours to be vented slowly, see section 6.4 "Water contamination in heat
transfer fluids", page 20.

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10. Conclusion
Heat transfer system maintenance is frequently ignored in the urgency to keep
production at high capacity. However, the heat transfer system is the backbone of the
production process and, as such, requires that operational and maintenance guidelines
be developed and followed to prevent unscheduled and excessive downtime, loss of
production and, ultimately, loss of revenue.

Good record-keeping of operational and maintenance data are the keys to avoiding
system problems, and to efficient troubleshooting when problems do occur; this
includes:
• routine fluid analysis,
• regular monitoring of system operation parameters,
• visual observation of system components, and
• a record of previous problems and their solutions.

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