Life time analysis of thermal oil used as heat transfer fluid in CSP power plant

H. Grirate, N. Zari, A. Elmchaouri, S. Molina, and R. Couturier

Citation: AIP Conference Proceedings 1734, 040005 (2016); doi: 10.1063/1.4949096

View online: https://doi.org/10.1063/1.4949096
View Table of Contents: http://aip.scitation.org/toc/apc/1734/1
Published by the American Institute of Physics

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 Life Time Analysis of Thermal Oil Used as Heat Transfer
Fluid in CSP Power Plant
H. Grirate1, 2, N. Zari1, a), A. Elmchaouri2, S.Molina3, R. Couturier3
1
Moroccan foundation for Advanced Science Innovation and Research MAScIR, Av med El Jazouli, Rabat,Morocco
2
Faculty of Sciences and Technology, LCPCB, University Hassan II Casablanca, Morocco
3
CEA LITEN, National Institute of Solar Energy, Thermal Systems Laboratory, Grenoble, France

a) n.zari@mascir.com

Abstract. The present work describes stability testing of hydrogenated terphenyl (HT), thermal oil available in the
market and considered as a potential HTF for CSP power plants. Before ageing tests, hydrogenated terphenyl was
compared to Biphenyl/diphenyl oxide (DPO) at the initial state, which is the most commonly used HTF in CSP plants
(SEGS VI and ANDASOL I) and included as a comparison material in the NREL HTF requirements. The (HT) stability
tests were performed in sealed ampoules (stainless steel) under inert gas blanket in the range of temperature between
250°C and 350°C (max temperature of HT) for 500 hrs. After ageing, many investigations were made to track the thermal
oil behavior after extended time over a range of temperature, such as chemical composition, flash point, viscosity, acid
value…. Laboratory testing indicated that the hydrogenated terphenyl (HT) is stable after ageing process at a temperature
of about 250°C. Nevertheless, it has shown signs of serious thermal cracking at elevated temperature which is reflected
by low flash point temperature. Therefore, the system must be purged effectively to purge the volatile decomposition
products.

INTRODUCTION
Various types of heat transfer fluids can be used in solar power plant (gas, oil, molten salts, steam…).
The selection of the best HTF is based firstly on the application temperature range to ensure the compatibility of the
fluid with the system.
As HTF, Molten salts reach the highest temperature (565°C) but they have high freezing temperature which
leads to complications in the collector field [2]. Steam is mostly used in Fresnel collector by the way heat
exchangers are avoided. Water is the most cost effective HTF and easy to control. Nevertheless, it is limited at a
temperature of about 100ºC when it starts to boil, becoming steam. Hence, it can only be used as a pressurized
system under imposing restrictions to ensure safe operation [3]. For an application such as system solar energy, a
high purity of water is required in order to prevent the corrosion phenomenon: this may increase the installation cost.
Selvakumar et al. [4] studied the heat transfer and fluid flow characteristics of various heat transfer fluids like
exceltherm, helium, calfo, therminol, duratherm, dynalene, molten salt and vegetable oil. Therminol was proposed
as the best heat transfer fluid for short flow length applications.
Synthetic oil is used as HTF in almost all commercial parabolic trough CSP plants. It is composed of a eutectic
mixture Biphenyl/diphenyl oxide (DPO) known under Therminol VP 1 or Dowtherm A. It has been successfully
operated in the majority of SEGS facilities for many years. By contrast to mineral oil, DPO exceed 312°C and can
reach up to 390°C. This organic HTF has a low melting point of 12° C, but exhibits a high vapor pressure at elevated
temperatures, approximately 10 bar at 390°C [5].
The formulation of the eutectic mixture is composed of 73.5% DPO and 26.5% biphenyl (Figure 1).

SolarPACES 2015
AIP Conf. Proc. 1734, 040005-1–040005-9; doi: 10.1063/1.4949096
Published by AIP Publishing. 978-0-7354-1386-3/$30.00

040005-1
 FIGURE 1.Components of Therminol VP-1/Dowtherm A

The most critical drawback of DPO is the relatively low boiling point (257°C). Even though the power
production of SEGS power plants was continuous and reliable for decades, significant heat losses have been
observed in a large number of receiver tubes. These losses have been assigned to the permeation of traces of
hydrogen gas through the steel tube wall into the vacuum around.
A number of studies have discussed the degradation of DPO and concluded that the working fluid has undergone
a pyrolytic decomposition at 400°C which led to the formation of a gaseous mixture that contained hydrogen, carbon
monoxide and aromatic hydrocarbons [6-7].
As alternative organic HTF, commercial formulations based on terphenyl-derived aromatics with high boiling
points (300-400°C) were proposed by several industrials. The hydrogenated terphenyl is one of the suggested fluids.
The objective of the experiment was to study the stability of the hydrogenated terphenyl commercially marked
under Therminol 66. The study is based on ageing fluid in the range of temperature between 250 and 350°C. In the
following section, a general description of the studied oil is given with the ageing procedure and characterization
methods. The results obtained are discussed later.

MATERIALS AND METHODS

Material Description
The substance is a commercial mixture of partial hydrogenated terphenyls (74–87%) (Figure 2), terphenyl (3–
8%), higher polyphenyls (18%) and quaterphenyl.
The fluid was purchased from its commercial source. Therminol 66 offers high temperature thermal stability and
is pumpable at low temperatures. The technical characteristics of this fluid are shown in Table 1 [8].

TABLE 1. Technical characteristics of the studied oil

Technical characteristics Therminol 66
Hydrogenated
chemical composition
terphenyl
Minimum working temperature 0°C
Maximum operating 345°C
temperature (liquid)
Maximum operating 375°C FIGURE 2. Component of Partially Hydrogenated
temperature (film) terphenyl
Density at 20 ° C 1008,1 kg/m3
Flash point 170°C
Auto-ignition 399°C
Pour point -32°C
Boiling point (1 bar) 359°C
Molecular weight 252 g/mol

Ageing Process
The test is undertaken in a closed system in the absence of oxygen in order to give a controlled environment. It
consists of metal ampoules (stainless steel) connected on the top with a purge inert gas (Argon) inlet/outlet to keep
oxygen out (1, 2 bar). A volume of 150 mL of tested oil was put into each ampoule which was sealed before inert
gas sparging.

040005-2
 Afterwards, the oil samples were exposed at temperatures of about 250 and 350°C for 500 hours. The
temperature was increased by 50°C increments every 24 hours and 5°C/hour at the last step until reaching the
desired temperature.

Characterisation Methods
Before ageing process, thermal stability was tested by therrnogravimetric analysis (TGA) from ambient to 400°C
at a constant heating rate of about 10°C/min. Approximately 20 mg of the tested oil was scraped and loaded onto a
platinum pan for testing. The sample was tested under nitrogen atmosphere at least twice, in order to observe the
evolution of the studied fluid during heat treatment in the absence of oxygen.
After ageing oils, various analysis methods were carried out to track the thermal oil behavior after extended time
over a range of temperature.
Fourier transformed infrared spectroscopy ABB Bomem Spectac FT-IR coupled to Attenuated total reflectance
(ATR) was used in chemical characterization from 500 to 4000 cm-1. The Gas chromatography–mass spectrometry
(GC-MS) analyses were made on an Agilent 7697A coupled to mass spectrometry in order to separate molecules.
Helium was used as carrier gas at a flow rate of 0.8 mL/min. The GC column was an HP-5 cross-linked with 5%
phenyl methylsi-loxane capillary column, 30 m × 250 µm × 0.25 µm. The column temperature was programmed at
70°C for 1 min, then 30°C/min to 150°C and then 10°C/min to 280°C, hold for 7 min until all peaks had eluted. The
injector and detector temperatures were set at 200°C. Data were acquired using Agilent Chemstation.
Oil viscosity was measured at 40°C using a Rheometer MCR 500. Other physical parameters (density, flash
point, acid number…) were measured using different techniques.

RESULTS ANALYSIS AND DISCUSSION

Therminol 66 before Ageing Process

Physical and Thermal Properties

Viscosity

Viscosity is a significant factor in heat transfer calculations. There is an inverse, close relationship between
viscosity and temperature: when the temperature increases, the viscosity decreases and vice versa. In addition, the
heat transfer fluid coefficient is greater when the potential for turbulence of the fluid is low.
The viscosity is also considered as an important criterion to assess the flow rate of a heat transfer fluid in CSP
power plant. Thus, the viscosity of Therminol 66 was plotted as a function of temperature in Figure 3 to be
compared with that of Therminol VP1.The values were extracted from the oils data sheets provided by Solutia [8-9].
Therminol VP 1 has a lower viscosity than Therminol 66 at low temperature. But even so, the VP1 suffers from a
freezing point around 12°C that requires heating during cold period, so more energy consumption [10].
The viscosity values of both oils show a similarity at high temperature.

Heat Transfer Coefficient

The ability to transfer heat is evaluated by the fluid heat exchange coefficient; it measures the thermal energy
that is transferred between the absorber wall and the fluid by convection. Many correlations have been proposed to
calculate the heat transfer coefficients in a circular tube. Each correlation depends on the flow regime: turbulent,
transitional or laminar.
In the case of a turbulent flow in a circular tube, the Reynolds number is equal to/or greater than 104. Thus, the
correlation (Dittus-Boelter) below is widely used [11]:
h= 0.023 (k/D) Re0.8 Pr0.4 (1)
Re : Reynold number = D.V.ρ/µ D : pipe diameter (m) V : Average velocity (m/s)
Pr : Prandlt number = Cp.µ/k ρ : Density (Kg/m3) Cp : Heat capacity (J/kg,K)
µ : Dynamic viscosity (Pa.s) k : Thermal conductivity W/m.K

040005-3
 3,5 1600
Therminol 66

Heat transfer exchange (W/m2.s)

3,0
Therminol VP1
Log (Dynamic viscosity) mPa,s

2,5 1400
2,0

1,5
1200
1,0

0,5
1000
0,0
Therminol 66
-0,5
Therminol VP1
-1,0 800
-50 0 50 100 150 200 250 300 350 400 200 250 300 350 400

Temperature °C Temperature (°C)

FIGURE 3. Dynamic viscosity of FIGURE 4. Heat transfer coefficient of

Therminol 66 vs Therminol VP1 Therminol VP1 vs Therminol 66

The heat transfer values are modeled from a 38 mm Inner diameter pipe with 1 m/s flow rate. The heat transfer
coefficient was calculated according to the equation (1). Figure 4 shows the plotted thermal exchange coefficients
of the two oils depending on the temperature.
It seems that the calculated heat transfer of Therminol VP1 is greater than Therminol 66. The plot also illustrates
a convergence since high temperature values. Although, the gap heat transfers in favor of TherminolVP1, there are
some physical limitations that can devalue its performance.

Vapor Pressure

Beside the importance bound to the heat transfer coefficient, the vapor pressure is a major requirement to avoid
the need to open the expansion tank [12]. This operation may lead to hot fluid contact with air which produces weak
acid formation. The above chart describes the vapor pressure of the compared thermal oils.
1000

Therminol 66
800
Therminol VP1
Vapor pressure kPa

600

400

200

50 100 150 200 250 300 350 400

Température °C

FIGURE 5. Vapor pressure of Therminol VP1 vs Therminol 66

Therminol VP1 exhibits clearly a higher vapor pressure than Therminol 66. A number of studies was discussed
that Therminol VP-1undergoes a gradual thermal breakdown when exposed to high operating temperatures [6-7]
which leads to generation of large volume of gases. In fact, the volatility of the samples increases with the high
concentration of light products [13].

040005-4
 Thermal Stability

TGA instrument has been used to evaluate the thermal stability of hydrogenated terphenyl (HT) for a better
understanding of the decomposition pathways that undergo the oil at the initial state.
The decomposition occurs on a single step under O2 atmosphere. Similar behavior is observed under inert gas.
Thus, the weight loss was defined at a temperature of about 300°C.The degradation occurs when the molecular
bonds break down.
Therminol 66 is a mixture of partially hydrogenated terphenyl. When exposed to a temperature higher than
250°C in a closed system, the fluid undergoes a slow cracking process. The mechanism reaction was proposed by
Schneider and Morgan [14] as follows:
- Decomposition in the absence of oxygen
The initiation reaction will probably consist of the elimination of a hydrogen atom from a cyclohexyl ring.
. .
(1) C6H11-C6H4-C6H11 C6H11-C6H4-C6H 10 + H

Then, the hydrogen atom would be extracted from another cyclohexyl or from a benzene ring.
. .
(2) C6H11-C6H4-C6H11 + H C6H11-C6H4-C6H 10 + H2
. .
(3) C6H11-C6H11-C6H5+ H C6H11-C6H10-C6H 4+ H2
Afterwards, the cyclohexyl ring radical (-C6H10) may undergo the following reaction (4):
. .
(4) C6H11-C6H4- C6H 10+ H C6H11- C6H4- C6H9 + H2

This reaction will be quite endothermic if the H atom had been removed from the position 2 on the ring, the
chain could break to produce cylohexane.
- Decomposition in the presence of the oxygen
The oxidative mechanism outlined for cyclohexane ring is based on schemes proposed by Semenov [15-17].The
general process is supposed to proceed via the reaction below:
. .
(5) C6H11-C6H4-C6H11 + O2 C6H11-C6H4-C6H 10 + HO 2
.
(6) C6H11-C6H4-C6H11 + O2 C6H11-C6H4-C6H10OO
.
(7) C6H11-C6H4-C6H10OO C6H11-C6H4-C6H9-COOH

The hydroperoxyde (C6H9OOH) will result in opening the cyclohexane ring. Thus, thermal oil oxidation
produces weak acid which can occur from contamination from external sources, presumably in open vent expansion
tank operation. It can be concluded that Therminol 66 may undergo decomposition at a temperature around 300 °C
in an open system. The presence of the oxygen can accelerate the reaction of the degradation which can limit the
fluid's service life. Therminol VP1 was tested in other studies and it have been demonstrated that the temperature of
degradation was deter-mined at 257°C [18]. This temperature is considered as a temperature of thermal boiling, a
value lower than the boiling point of Therminol 66 (359°C). In this case, more vapors are generated by Therminol
VP1 causing then a pressure in-crease.

Therminol 66 after aging process

Sample Appearance

The tested samples were recovered and pictured in order to show the color changes that the oil went through
during the ageing process. As shown in Figure 6, the thermal oil has changed color and becomes more yellowish as
a function of temperature after 500h of ageing.

040005-5
 FIGURE 6. Samples oils aged at 350°C

Chemical Analysis

The Figure 7 presents the spectrum of Infrared spectra of tested oil. Fourier transform infrared spectroscopy
(FTIR) is considered as an important analysis technique which detects various characteristic functional groups
present in the oil [19]. Under the current ageing conditions, no detectable oxidation was demonstrated. The carbonyl
and the hydroxyl bands (1750- 3600cm-1) are absent in the analyses. The curves show only the oil structure. Hence,
the synthetic oils chemical composition has not undergone any change after ageing process.
The GC-MS analysis of the oil samples was carried out to identify the compounds present in the oil. The
chromatograms obtained are presented in Figure 8 and the compounds analyzed are summarized in Table 2. It has
been observed that the tested oil contains several compounds. Taking into account the area percentage, the highest
peak areas of total ion chromatogram were: cyclohexylbiphényl (236 g/mol), dicyclohexylbenzène (242 g/mol), and
terphenyl (230 g /mol). The compounds present in hydrogenated terphenyl are mostly aromatic hydrocarbons with
carbon number ranged from C11 to C24.

Csp2-H
aromatic
Csp3-H Csp2-H
C=C
m- disutitued
aromatic
aromatic
T66 initial state
T66 250°C Csp2-H monosubtitued
T66 350°C aromatic
4000 3500 3000 2500 2000 1500 1000 50
No (cm-1)

FIGURE 7.Therminol 66 Infrared spectra

12
T66 initial state 8 13
T66 250°C 6
11
T66 350°C 9
10
7
5 15
14
2 3 4 16

15

2 16
3 4

2
1
3 4 15 16

3 4 5 6 7 8 9 10 11 12 13 14 15 16

Retention time (min)

FIGURE 8. Hydrogenated terphenyl chromatograms

040005-6
 TABLE 2. Quantification of the peak areas present in the GC-MS chromatogram
% peak areas
Retention
Molecular Chemical HT HT at HT at
Peak time Compounds Name
weight (g/mol) formula Initial state 250°C 350°C
(min)
1 4,58 146 C11H14 Benzene, cyclopentyl- 0 0 0,5

2 5,34 160 C12H16 Benzene, cyclohexyl- 0,6 0,3 0,8

3 6,41 172 C13H16 3Benzene, 2 heptynyl 0,2 0,1 0,1

4 Anthracène 0,1 0,09 0.06

9,25 186 C14H10

5 10,66 236 C18H20 Cyclohexylbiphényl 1,8 1,4 1

6 10.95 230 C18H14 terphenyl 6 5,6 7,2

7 11,22 236 C18H20 Cyclohexylbiphényl 3,4 2,6 0,2

8 11,96 242 C18H26 dicyclohexylbenzène 11 10 8

9 12 ,10 242 C18H26 dicyclohexylbenzène 7,3 7,1 5,3

10 12,32 236 C18H20 Cyclohexylbiphényl 7,4 7 6,7

11 12,41 242 C18H26 dicyclohexylbenzène 7,4 7,4 7,4

12 12,79 236 C18H20 Cyclohexylbiphényl 12,7 12,3 12,2

13 13,19 236 C18H20 Cyclohexylbiphényl 9 10 9

14 13,38 230 C18H14 terphenyl 1,2 1,2 1,3

15 15,08 240 C18H24 1-Phenyl-2-cyclohexylcyclo-1-hexene 2 1,8 0,16

15,55 306 C24H18 0,4 0.5 0.4

16 Quaterphenyl

Analyses by FTIR and GC-MS have shown that Therminol 66 is composed from:
230 g/mol: terphenyl 236 g/mol: Cyclohexylbiphényl 242 g/mol: dicyclohexylbenzène

According to the above table, it appears that the percentages of the calculated areas decrease in function of the
temperature with the exception of the peaks attributed to the terphenyl (230g / mol) and benzene-cyclohexyl (160 g /
mol) which presents minor percentage.
Indeed, when increasing the temperature, thermal oil produces more gases due to its chemical reactions
occurring at high temperature which causes rearrangement of the molecules present. For example: the
dehydrogenation reaction, corresponding to the loss of hydrogen. When cyclohexylbiphenyl loses hydrogen, it
stabilizes in terphenyl. Hence the reaction corresponding to the increase in percentages of peak areas related to
terphenyl is described as follows:

Hydrogen (H2), cyclohexene (C6H10) benzene (C6H6), cyclohexane (C6H12) are among the gas or light
compounds that may be generated during the ageing of the oil T66.These compounds can be obtained due to thermal

040005-7
cracking of the molecules present in the oil. Thus, the composition of the oil did not change at high temperature.
However, the intensive release of light compounds can reduce the amount of available oil in the installation.

Physical Measurements

Table 3 shows the measurements made in order to assess the behavior of the aged oils. As the thermal fluid is at
high temperature, the risk of fire is always present. Among the measurements of fire safety in thermal fluid systems,
there is Flash point. It’s defined as the lowest temperature when the liquid generates vapors which ignite in the
presence of an external ignition source and oxygen.
The fluid has indicated signs of serious thermal cracking at temperatures of about 350°C. This phenomenon is
reflected by the low flash point temperature which reveals highly volatile decomposition products. A further
parameter that was assessed is viscosity at a temperature of about 40°C which represents a change in the fluid’s
molecular sizes. Interestingly, the viscosity has marked a significant decrease from 32 to 23 mPa.s, which confirms
the presence of volatile products. In fact, the dropping of the flash point temperature and the viscosity indicates that
the system is not vented effectively. As a result, the decomposition volatiles products are starting to accumulate in
the oil [20]. Total acid number (TAN) is considered to be an important indicator for thermal oil quality, especially to
identify oxidation states. If the acid number is determined out of specification, it is strongly recommended to replace
the heat transfer fluid. The average of a new material acid number is situated between 0 and 0.1. When the acid
number exceeds 0.5, corrective action must be taken to avoid the oxidation problem [21].Indeed, the presence of
oxygen in high heating process leads to its combination with hydrocarbons structures. This reaction may lead to the
formation of carbonyl containing products. The oxidation products increase the fluid thickness, which leads to a
viscosity rise [22].For the oil samples studied here, the acid number measurement has revealed that no oxidation
phenomenon has occurred. This result is confirmed by the absence of the carbonyl and hydroxyl bands in the
infrared spectrum (Fig.7). Furthermore, the viscosity has shown a decrease after the heating process. This is due to
condensation of light products which can indicates that the system is not vented effectively.

TABLE 3. Physical Measurements of Tested Oils

Viscosity at Flash Point Density Acid number Water

Synthetic Oils (g/cm3) (mgKOH/g) Content (%)
40 °C (mPa.s) (°C)

T66 initial state 32 178 1,02 0 0

250°C Aged HT 33 178 1,05 0 0
350°C Aged HT 23 78 1,03 0 0

CONCLUSION
According to the comparison performed at the initial state, Therminol VP1 has high heat transfer efficiency
compared to Therminol 66. However, a major requirement when selecting a new heat transfer fluid is a low vapor
pressure, to avoid opening the expansion tanks, as well as a low freezing point to prevent the pipe clogging.
Therminol VP1 has a high freezing point around 12°C that requires heating operations during cold periods and a
vapor pressure of 10 bars at 390°C. Also, Therminol VP1 generates more gases than Therminol 66, these gases lead
to significant heat losses in the receiver tubes.
The ageing of a heat transfer fluid (HTF) is a complicated chemical process [24], even though, hydrogenated
terphenyl samples were thermally aged at a temperature between 250°C and 350°C during 500 hours under argon
atmosphere into stainless steel ampoules hermetically closed. The accelerated process revealed that the aged T66 at
350°C has undergone a thermal cracking which leaded into their arrangements of molecules as well as the
generation of light products. Typically, when a heat transfer fluid deteriorates, it forms volatile products which
lower the flash point, and heavy products which increase the viscosity and thus lower the heat transfer coefficient.
Nevertheless, the viscosity of the HTF has dropped after ageing which indicates that the system is not vented
effectively.

040005-8
 In conclusion, all organic chemical structures undergo thermal degradation as heat is applied but it differs by the
degree of deterioration. Depending on the fluids vapor pressure, Therminol 66 generates less light products than
Therminol VP1. Hence, it remains as a competitor fluid to be used as heat transfer fluid in CSP power plant.

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