A Final Stage Presentation on

EVALUATION OF FIRE RESISTANT HYDRAULIC FLUID TO

REPLACE CONVENTIONAL MINERAL OIL IN NUCLEAR
INDUSTRY
Presented by

Zeeshan Ahmad
(132090007)
Under the Guidance of

Dr. V.M.Phalle
Associate Professor & TPO

VEERMATA JIJABAI TECHNOLOGICAL INSTITUTE

(An Autonomous Institute Affiliated to University of Mumbai)
Mumbai 400019
&

Mr. N. L. Soni, OS /Mr. P. K. Mishra, SO/E

REFUELLING TECHNOLOGY DIVISION
Reactor Design & Development Group
Bhabha Atomic Research Centre

 Contents
1. Introduction
. Problem definition
. Objective
. Summery

2. Literature review
. Classification of Hydraulic Fluids
. Classification of Fire-Resistant Hydraulic Fluids, Their Properties and Uses
. Properties of Hydraulic Fluids and Their Effect on System Performance
. Requirements for Fire-Resistant Hydraulic Fluids
Tribological Properties of Hydraulic Fluids
Effect of Gamma Radiation on Properties of Hydraulic Fluid

3. Methodology
. Tribological Evaluation of Hydraulic Fluids
. Gamma Irradiation of Hydraulic Fluids

4. Discussion and results

5. Conclusion and future scope
6. References

1.Introduction
1. Objective
. Study of different types of hydraulic fluids and their properties and selection of fire
resistant hydraulic fluid based on previous data available and system requirements.
. Study of tribological behaviour of different hydraulic fluid and selection of standard
method of evaluating tribological properties based on our requirements.
. Conclusion based on experimental data of both the hydraulic fluids.
. Preparation and submission of report on tribological behaviour of hydraulic fluids.
. Planning and preparation of sample for gamma radiation of hydraulic fluids inside a
gamma chamber located at ISOMED, south side of BARC.
. Measurement of viscosity, viscosity index of radiated oil samples at different
temperatures and conclusion based on experimental data.

2. Summery
a) Literature Reviewed
) Study of different types of hydraulic fluids
) Selection of fire resistant hydraulic fluid
) Study of properties of hydraulic fluids and their effect on system performance
) Study of different tribological test methods as per ASTM and ISO
standards
) Study of effect of gamma radiation on properties of hydraulic fluids

2.Literature Survey
Sr.
No.

Author Name & Book Title

Literature

Engineering
Design Classification
of
Hydraulic
Handbook
of
Hydraulic Fluids , Tribological Properties
Fluids, Headquarters, U.S. of Hydraulic Fluids
Army Materiel Command,
April 1971.

Lubricants, Industrial Oils Fire-Resistant Hydraulic Fluid

and Related Products (Class Types
for
Industrial
L) Classification Part 4: Applications
Family
H
(Hydraulic
Systems),
ISO
Standard
6743

Hydraulic Fluid Power Fire- Requirements

for
FireResistant
(Fr)
Fluids
Resistant Hydraulic Fluids
Guidelines for Use, Bureau
of Indian Standards, New
Delhi-110002.

H.
H.
Zuidema,
The Friction, Wear, and
Performance of Lubricating Lubrication: Terms and
Oil,
Reinhold
Publishing Definitions

Sr. No.

Author Name & Book Title

Literature

S. Sharma, S. Sangal, K. Mondal,

On the optical microscopic
method for the determination of
ball-on-flat
surface
linearly
reciprocating
sliding
wear
volume, Wear 300 (2013) 82
89

Measurement and Calculation of

Wear, A model for calculation of
the wear volume in case of linearly
reciprocating sliding wear test has
been studied in this paper to get
accurate and quick results. The
model proves to be an effective
tool for the calculation of the wear
volume.

Charles Spar, Hydraulic Fluids Relative radiation resistance

and Their Applications, ASME various hydraulic fluids.
Publication 64 WA/LUB-14.

R.O .Bolt and J.G. Carrol, Effect Change of properties of lubricant

of
radiation
on
aircraft because of gamma irradiation
lubrications
and
fuels,
California Research Corporation,
WADC Technical Report No 56646, Part II, ASTIA Document
No. AD 151176. April 1958.

Zeeshan Ahmad, P.K.Mishra, Tribological

data
of
gamma
Determination of Effect of irradiation on hydraulic fluids.
Gamma Radiation on Petroleum
based Hydraulic Fluid - ENKLO68 RTD Report, BARC, Mumbai

of

Literature Survey conti..

Sr.
No.

Bench Type
Wear Tester

Friction

and Literature

Timken Tester
Federal Test Method 6505

A steel block is pressed against a

rotating, cylindrical steel ring

Almen Tester

a cylindrical rod is rotated in a split

bushing which is pressed against it

Falex Tester
Federal Test Method 3807
Federal Test Method 3812

A cylindrical rod is rotated between

two hard V-shaped bearing blocks
which are pressed against the rod

&

Four-ball Tester
ASTM D-2596-67T,
Federal Test
Method 6514 & ASTM D-2266-64T

In the four-ball machine (often called

the "Shell" Four-ball Tester) a 1/2-in.diameter steel ball is rotated in contact
with three stationary similar balls
which are clamped in a fixed position

SAE Tester
Federal Test Method 6501

In the SAE machine, two cylinders

aligned axially and in contact with
each other are driven at different
speeds. One of the cylinders may be
driven in either direction. The pieces
revolve under a flooded lubrication
condition from the test liquid held in a
cup.

ASTM
Designation
G13305(2010), Standard Test Method
for Linearly Reciprocating Ball-onFlat
Sliding
Wear,
ASTM

A flat specimen and a spherically

ended specimen (here in called the
ball specimen), which slides against
the flat specimen. These specimen

Bench Type Friction and Wear Tester

3.Methodology
1. Tribological testing of hydraulic fluid
. Objective:
.
.
.

The main objectives of this test was

To evaluate the wear characteristics hydraulic fluids at different conditions
To compare these wear characteristics of the two oil samples with each
other

. Apparatus and materials:

.
.
.

This test has been carried out at Refueling Technology Division (RTD), BARC
Mumbai
A reciprocating sliding wear and friction machine (Plint and Partner TE-70)
was used based on ASTM G133 Procedure B
Bearing steel plate SS-52100 and bearing steel balls SS-52100 of 1/2 inch
(12.7 mm) diameter were used as fixed specimen and moving specimen
respectively.

Other test conditions:

Oil

Temperature

Name

(C)

Oil-A
FRHF

65

POE
Oil-B
Mineral

65

Oil-A
FRHF

90

POE

Test Procedure:

Load(N)

Frequency

Sliding

Stroke

Time

(Hz)

Distance

Length

(Sec)

(M)

(MM)

15
15

10
20

400
400

1
1

20000
10000

25
15
15
25
15
15

10
10
20
10
10
20

400
400
400
400
400
400

1
1
1
1
1
1

20000
20000
10000
20000
20000
10000

25

10

400

20000

 The following test procedure was followed as per

ASTM standard G133 05
1. Specimens on which experiments were carried out (e.g. plate &
ball) were cleaned thoroughly using acetone and ultrasonic
cleaning machine. The samples were dried by using hot air.
2. The sample bath was cleaned using acetone & was dried with hot
air.
3. The specimens were cleaned after they were secured in place in
the test fixture by wiping with acetone and then with lint free
tissue paper.
4. The ball specimen was gently lowered upon the flat specimen & it
was also ensured that the reciprocating drive shaft motion was
horizontal & parallel to the surface of flat specimen.
5. The test load was applied. It was confirmed that the desired
oscillating speed had been set before starting the test

 Test Parameters:
Sr.
No.
1
2
3
4

Parameter
Applied Normal ForceBall Tip Radius
Stroke Length
Test Duration

As
per
ASTM
( Procedure B)
200 N
4.76 mm
10 mm
sliding Distance 400 m

Frequency of oscillation

10 Hz

Type of motion produced Not Specified. It can be Sinusoidal

by the oscillating drive velocity profile, triangular velocity
system
profile

Sinusoidal velocity
profile

Ambient
relative 40 to 60 %
humidity
Ambient Temperatures
150 2C
Medium
Lubrication

60%

8
9

Standard Parameters
Used
For This Test
15 N, 25 N
in (12.7 mm)
1 mm
sliding Distance 400
m
10,20,10 Hz

65C
Lubrication

 Measurement and Calculation of Wear:

1. Wear measurement of ball specimen:

.
.

Owing to the nature of this type of test, the wear on ball specimen may not
be circular or flat always therefore refer the following which applies.
If the ball appears flat but not circular, the average of the maximum and
minimum dimensions of the scar is taken as effective ball scar diameter
(D).
Pin scar measurement may be made by removing the ball specimen holder
and placing the wear scar portion under the microscope. A calibrated
ocular or a photo-micrograph of known magnification may be used to
measure scar dimensions.

As per ASTM G99-05(2010) Volume loss of Ball in mm3 is calculated using

following formula

Where Vb= Wear volume for ball scar of diameter D in mm3

D = Ball scar diameter in mm
R = Ball radius in mm
Note: This is an approximate geometric relation that is correct to 1 % for (wear scar diameter/ball radius)
<0.3, and is correct to 5 % for (wear scar diameter/ball radius) <0.7. The exact equation is as given below.

Volume loss of ball (Vb) is given by,

Where
D = Wear scar diameter
R = Radius of Ball
Wear rate of ball is calculated using following formula.

Where k = Wear rate of ball in mm3/Newton.

Meter
Vb = Wear volume for ball scar of diameter D in mm3
P = Load in N
L = Sliding Distance in mm

2.
Wear of Flat specimen:

Wear of Flat specimen is calculated using following formula

Where, w = width of wear scar in mm
d = depth of wear scar in mm
l = length of wear scar in mm

Typical photographs indicating Ball wear

Typical photographs indicating Plate wear

Plate SS-52100, 15 N, 10 Hz, 20000 sec

Plate SS-52100, 25 N, 20 Hz, 10000 sec

 Results and Discussion

1. Effect of Temperature on Coefficient of Friction
Stribeck Curve for OIL-A and OIL-B
0.11
OIL-A
0.1

OIL-B

Coefficient of Friction
0.09
0.08
0.07

Re gime Regim
1
e2

0.06

Re gime 3

0.05
0

0.05

0.1

0.15

0.2

*V/P(Stribeck Parameter)

0.25

0.3

0.35

Friction Characteristics
Effect of Temperature on Coefficient of Friction
15 N / 20 Hz

Effect of Temperature on Coefficient of Friction

15 N / 10 Hz
0.09

Coefficient of Friction
0.08

0.08

Oil-A

0.09 0.09

0.08

0.08

Oil-B

0.1

0.1
0.1

0.09

0.1

Oil-A
0.1

0.09

0.07

Coefficient
of Friction
0.08

0.06

0.06

0.05
27

65

0.05

90

27

Temperature (C)

Temperature (C)

Effect of Temperature on Coefficient of Friction

25 N / 10 Hz
0.1
Coefficient
of Friction
0.09
0.08

OilA

0.09 0.09

0.08
0.07

0.07

0.07
0.06
0.05
27

65

Temperature (C)

65

90

90

Oil-B

 Wear Characteristics
1. Ball Wear
Load Vs. Wear Rate of Ball
27C /10 Hz

10

1.50 -7
1.20
0.90

OILA

1.20

0.83

Wear Rate(mm/Nm)
0.60

0.38

0.36
0.30

Load Vs. Wear Rate of Ball

65C /10 Hz
1.50

0.00
15

Load (N)

OILA

25
1.20
0.90

0.87

0.86

Wear Rate(mm/Nm)
0.60
0.30

0.22

0.21

0.00
15

Load (N)

25

 Plate Wear
6.00

Load Vs. Wear Rate of Plate

27C /10 Hz
OILA

4.79

5.00
4.00
3.00

2.82

Wear Rate(mm/Nm)
2.00

1.81
1.36

1.00
0.00
15

Load (N)

25
5.00

Load Vs. Wear Rate of Plate

65C /10 Hz
OILA

4.00

3.53

Wear Rate(mm/Nm)
3.00
2.21
2.00
1.00

1.45
0.56

0.00
15

Load (N)

25

2. Radiation resistance of hydraulic fluid

. Objective:
.
.
.
.

The main objectives of this test was

To give a brief description of fluids and standard test methods for viscosity
measurement.
To measure the viscosities of the Radiated oil sample at different level of
radiation.
To compare the result of two different oil sample each radiated at five
different levels of radiation.

Sample Preparation

 Measurement of properties of ENKLO-68:

1. Density:
Following graph gives the variation of density in g/cm 3 for fresh as
well as irradiated oil samples with respect to temperature in
range of 15-100 C (288K to 373K).

0.90
0.80
0.70

Density (g/cm)

Density Vs Temperature

0.60

0 Mrad (Fresh Oil)

5 MRad
25 MRad
50 MRad
100 MRad
300 MRad

0.50
0.40
0.30
0.20
283

303

323

343

Temperature (K)

363

383

2. Effect of Gamma Radiation on Kinematic

Viscosity:
Following graph gives the variation of Kinematic Viscosity in
mm2/s (cST) for fresh as well as irradiated oil samples with
respect to temperature in range of 15-100 C (288K to 373K).
1000.0

Kinematic viscosity Vs Temperature

0 MRad (Fresh Oil)
5 MRad
25 MRad
50 MRad
100 MRad
300 MRad

100.0

Kinematic Viscosity (mm2/s)

10.0

1.0
283

303

323

Temperature (K)

343

363

383

3. Effect of Gamma Radiation on Viscosity index:

110
100
90
80

Viscosity index
70
60
50
0

50

100

150

200

250

Gamma Radiation Dose (MRad)

300

350

Measurement of properties of POE-68 oil:

1. Density:
Following graph gives the variation of density in g/cm 3 for fresh as
well as irradiated oil samples with respect to temperature in
range of 15-100 C (288K to 373K).

Density (g/cm)

Fresh
5 MRad
25
MRad
0.2
283

303

323
343
Temperature (K)

363

383

2. Effect of Gamma Radiation on Kinematic

Viscosity:
Following graph gives the variation of Kinematic Viscosity in mm2/s
(cST) for fresh as well as irradiated oil samples with respect to
temperature in range of 15-100 C (288K to 373K).
Viscosity Vs Temp Graph for POE oil
500
Fresh
5 MRad
25 MRad
50 MRad

Viscosity mm/s

100 MRad
300 MRad

50

5
270

290

310

330

Temperature K

350

370

3. Effect of Gamma Radiation on Viscosity index:

150
148

Viscosity Index

146
VI

144
142
0

50

100

150

200

250

300

Gamma Radiation Dose (Mrad)

Fresh
Oil
Sample

5
MRad

25
MRad

50
MRad

100
MRad

300
MRad

4. Conclusion and Future Scope

5. Tribological Evaluation
.

The tribological evaluation for qualifying hydraulic Oil-A and Oil-B has been
done on sliding friction and wear machine TE-70. Friction and wear were
the major candidate for qualifying the oils.
As discussed in previous chapter, the friction characteristics of the two oils
are almost same. The stribeck curve shows that both Oil-A and Oil-B have
similar operating conditions in hydrodynamic regime.
The wear characteristics shows that the wear rate of ball and plate under
Oil-A lubrication is high as compared to Oil-B but the order of wear rate is
very low for both oils and is of order 10-7, which is condition of mild wear.
Hence it can be acceptable.
Based on tribological experiment it can be concluded that both hydraulic
oils are similar in tribological behaviour, Oil-A has the advantage of being
fire resistant. There for Oil-B can be replaced by Oil-A if there is chances of
fire hazard or the operating temperature is high.

2. Radiation Resistant
. There is approx. 5.92% decrease in the density of the ENKLO 68 and 6.02%
decrease in the density of the POE 68 from 15 to 100 C
. The density of both ENKLO-68 and POE-68 oil has been found to be resistive to
radiation levels up to 300 MRad for same temperature as the radiation level
increases Density is not much affected.
. The viscosity of the ENKLO-68 has been found to be more resistive to radiation
levels and is affected by 12-13% only where as POE-68 oil has been found to be
less resistive and is affected by 50-60% for same temperature.
. It is found that the percentage change in viscosity for both oil samples is higher in
lower temperature range as compared to that in higher temperature range with
respect to un-irradiated fresh oil sample.
. The viscosity index of the ENKLO-68 oil has not improved because of radiation
and remains constant, where as VI of POE-68 oil has improved.
. The appearance of hydraulic oil ENKLO-68 has changed after exposure to Gamma
radiation, where as the appearance of hydraulic oil POE-68 Remains unchanged.
. Analysis of Total Acid Number (TAN) and Total Base Number (TBN) may give the
change in acidic or basic content in the oil. This may be helpful to decide the
effect of irradiated oil on the components of hydraulic system.

Based on above discussion it is concluded that up to 50 MRad radiation

level Oil-A can be used as hydraulic fluid in replacement of Oil-B in nuclear
industry when the operating temperature is high.

Future Scope

The test procedure discussed in this report for sliding friction and wear
measurement can be used for general purpose friction and wear test under
lubricated or dry condition.
The data available in this report can be used for selection of hydraulic oils
for other applications also.
The properties of hydraulic oils will required to be evaluated at more
radiation levels, for this purpose it is planned to irradiate hydraulic oils at
5, 25, 100, 200, 300, 400 and 600 MRad radiation levels.
The appearance of oil is not a major concern in this report but in future the
oil has to be further analysed for presence of oxidation compounds using
TAN and Oxidation Stability test.
Change-over of a system from one hydraulic oil to another can create
problems unless consideration is given to circuit and component design.
For this purpose, a Fire Resistant Hydraulic Fluid Test Facility (FRHTF) will
be developed by RTD at Engineering Hall 3. In this facility hydraulic
performance, compatibility with existing hydraulic components, and high
temperature operability will be tested by evaluating the changes in
properties of the hydraulic oils after being used in this facility test setups.
The test facility will be designed to be operated without any operator.
A man machine interface (MMI) will be required to design to run this test

References
1.Engineering Design Handbook of Hydraulic Fluids, Headquarters, U.S. Army Materiel Command, April 1971.
2.W.D. Phillips, A Comparison of Fire-resistant Hydraulic Fluids for Hazardous Industrial Environments. Part 1. Fire resistance and lubrication
properties, FMC Corporation (UK) Ltd.
3.Sullivan, M.V., Wolfe, J.K., and Zisman, W.A., Flammability of the higher boiling liquids and their mists, Zng. Eng. Chem., 39, 12 (1947), 160714.
4.Murphy, C.M., and Zisman, W.A., Synthetic hydraulic fluids, Product Engineering, 21, 9 (1950), 109-13.
5.Lubricants, Industrial Oils and Related Products (Class L) Classification Part 4: Family H (Hydraulic Systems), ISO Standard 6743.
6.Santosh Javalagi and Swaroop Reddy Singireddy, Hydraulic fluid properties and its influence on system performance, Linkping University.
7.Hydraulic Fluid Power Fire-Resistant (Fr) Fluids Guidelines for Use, Bureau of Indian Standards, New Delhi-110002.
8.Friction, Wear, and Lubrication: Terms and Definitions, Research Group on Wear of Engineering Materials, Organization for Economic
Cooperation and Development.
9.H. H. Zuidema, The Performance of Lubricating Oil, Reinhold Publishing Corp., N. Y., 1959.
10.
Federal Test Method Standard No. 791a, Test Method No. 6505.
11.
Federal Test Method Standard No. 791a, Test Method No. 3807.
12.
Federal Test Method Standard No. 791a, Test Method No. 3812.
13.
ASTM Standards 1969, Designation D-2596- 67T, Part 17, p. 970, Philadelphia, American Society for Testing Materials, 1969.
14.
Federal Test Method Standard No. 791a, Test Method No. 6514.
15.
ASTM Standards 1967, Designation D-2266- 64T, Part 17, p. 799, Philadelphia, American Society for Testing Materials, 1967.
16.
Federal Test Method Standard No. 791a, Test Method No. 6501.
17.
H. Gisser, The Effects of Nuclear Radiation in Lubricants, Conference on Effects of Nuclear Radiation on Materials, Watertown Arsenal, 1967.
18.
R. C. Gunderson and A. W. Hart, Synthetic Lubricants, Reinhold Publishing Corp., N.Y., 1962.
19.
Roger E. Hatton, Introduction to Hydraulic Fluids, Reinhold Publishing Corp., N. Y., 1962.
20.
Charles Spar, Hydraulic Fluids and Their Applications, ASME Publication 64 WA/LUB-14.
21.
R.O .Bolt and J.G. Carrol, Effect of radiation on aircraft lubrications and fuels, California Research Corporation, WADC Technical Report No 56646, Part II, ASTIA Document No. AD 151176. April 1958.
22.
William L. R. Rice, Nuclear Radiation Resistant Lubricants, California Research Corporation, WADC Technical Report No 57-299, ASTIA Document
No. AD 118329 May 1957.
23.
S. Sharma, S. Sangal, K. Mondal, On the optical microscopic method for the determination of ball-on-flat surface linearly reciprocating sliding
wear volume, Wear 300 (2013) 8289
24.
ASTM G133-05(2010), Standard Test Method for Linearly Reciprocating Ball-on-Flat Sliding Wear, ASTM International, West Conshohocken, PA,
2010,www.astm.org
25.
Zeeshan Ahmad, P.K.Mishra, Determination of Effect of Gamma Radiation on Petroleum based Hydraulic Fluid - ENKLO-68 RTD Report, BARC,
Mumbai
26.
http://www.viscopedia.com/methods/measuring-principles/
27.
Hutchings, I.M. (1992), Tribology Friction and Wear of Engineering Materials, Edward Arnold, London.
28.
Zum Gahr, K.-H. (1987), Microstructure and Wear of Materials, Tribology Series 10, Elsevier, Amsterdam.