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STP 1021
Turbine Oil Monitoring
William C. Young and Reginald S. Roberton, editors
ASTM
1916 Race St.
Philadelphia, PA 19103
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Library of Congress Cataloging-in-Publication Data
Turbine oil monitoring/William C. Young and Reginald S. Roberton,

editors.
(STP ; 1021)
Papers presented at the symposium held in Orlando, FL on 8 Dec.
1987 and sponsored by ASTM Committee D-2 on Petroleum Products
and Lubricants.
"ASTM publication number (PCN) 04-01021012"--T.p. verso.
Includes bibliographies and index.
ISBN 0-8031-1252-1
1. Turbomachines--Lubrication--Congresses. I. Young, William C.
II. Roberton, Reginald S. III. ASTM Committee D-2 on Petroleum
Products and Lubricants. IV. Series: ASTM special technical
publication; 1021.
TJ266.T873 1987
621.406--dc19 89-301
CIP
Copyright 9 by AMERICAN SOCIETY FOR TESTING AND MATERIALS 1989
NOTE
The Society is not responsible, as a body,
for the statements and opinions
advanced in this publication.
Peer Review Policy
Each paper published in this volume was evaluated by three peer reviewers. The authors
addressed all of the reviewers' comments to the satisfaction of both the technical editor(s)
and the ASTM Committee on Publications.
The quality of the papers in this publication reflects not only the obvious efforts of the
authors and the technical editor(s), but also the work of these peer reviewers. The ASTM
Committee on Publications acknowledges with appreciation their dedication and contribution
of time and effort on behalf of ASTM.
Printed in Baltimore, MD
April 1989
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Foreword
This publication, Turbine Oil Monitoring, contains papers presented at the symposium of
the same name held in Orlando, Florida on 8 Dec. 1987. The symposium was sponsored by
ASTM Committee D-2 on Petroleum Products and Lubricants. William C. Young, General
Electric, and Reginald S. Roberton of Princeton, New Jersey presided as symposium co-
chairmen and were coeditors of this publication.
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Dedication
This book is respectfully dedicated to Andrew N. Smith and Reginald S. Roberton in
recognition of their years of effort as, respectively, chairman and secretary of Subcommittee
D02.C on Turbine Oils. In their offices they promoted, both in the United States and
internationally, greater knowledge of turbine lubrication and the use of ASTM standards
to improve turbine lubrication performance. ASTM D 4378, "Practice for In-Service Mon-
itoring of Mineral Turbine Oils for Steam and Gas Turbines," the focus of this symposium,
was the result of their dedication.
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Contents
Overview
Background and Development of ASTM D 4378: Practice for In-Service

Monitoring of Mineral Turbine Oils for Steam and Gas Turbines---
R. S. ROBERTON 3
A Turbine Lube Oil System Monitoring Program~D. BONETT 19
A Supplier's Approach to Turbine Oil Monitoring---G. R. TRABERTAND

G. J. SCHREUDERS 25
The Reliable Control of Oil Quality in Japanese Turbine Units---

R. OHGAKE, M. SUNAM1, T. YOSHIDA, AND H. WATANABE 32
Monitoring Practices for Phosphate Ester Fluids for Turbine Lubrication

and Control---J. F. ANZENBERGER,SR. 44
Experiences with an Analytical Monitoring Program Designed for

Commerical Flight Tests of Advanced MiI-L-23699 Turbine Fluids--
D. G. PACHUTA, J. A. THICH, R. W. KNIPPLE, AND D. A. STEPHANIC 54
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STP1021-EB/Apr. 1989
Overview
ASTM D 4378, Practice for In-Service Monitoring of Mineral Turbine Oils for Steam and
Gas Turbines, was developed by Subcommittee D02.C on Turbine Oils in response to the
needs of the electrical power generation community. The organizations for which this doc-
ument is intended are the utilities and industries which generate their own electrical power.
The purpose of D 4378 is to recommend:
1. Which tests to run.
2. The frequency of testing.
3. The interpretation of the results.
4. Corrective actions.
5. Limiting values.
This symposium brought together suppliers and consumers to present their views on
turbine fluid monitoring.
An overview was presented by Roberton giving the user needs that generated D 4378.
The history of the document was discussed with the reasons for having the tests which are
included, the basis for interpreting the results, and the appropriateness of the limits.
The necessity for a monitoring program was brought forth by Bonett, who presented the
experiences of an American utility. These show that a program can identify problems so
that corrective action can be taken in time to prevent a major shutdown.
The views of an American lubricant supplier were given by Trabert and Schreuders, who
stressed the need for close cooperation between the turbine operator, the turbine manu-
facturer, and the lubricant supplier to ensure the successful operation and effective moni-
toring of a turbine circulating system.
Ohgake and his associates reported on the technological revolution in Japan since 1955.
Maximum unit capacity has increased from 66 M W in 1955 to 1000 MW in 1987. A t the
same time, steam pressure of 60 kg/cm 2 in 1955 has risen to 246 kg/cm 2 with a corresponding
rise in steam temperature from 480~ to 566~ Turbine oil operating temperatures increased
by 10 to 15~ thereby potentially more than doubling the oxidative degradation rate of the
lubricant.
Ohgake confirmed the use of ASTM D 2272 in their monitoring programs and for the
calculation of turbine severity, and also indicated that the concept of regular makeup (re-
placing part of the oil charge) to compensate for oil degradation was still considered a useful
practice to ensure long oil service life. In Japan and in the United States, increased demands
have been placed on turbine lubricating oils by changes in the design of the turbine gen-
erators. The increased use of combined cycle stations has added the requirement that the
same lubricant be used in both gas and steam turbines. (In a combined cycle installation,
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2 TURBINE OIL MONITORING
heat recovered from the gas turbine exhaust is used to help generate steam for driving a
steam turbine.) These new demands on the oil have made monitoring programs even more
important than previously.
Although D 4378 addresses the more commonly used petroleum oil turbine lubricants,
fire-resistant fluids based on phosphate esters are increasingly being used for electrohydraulic
control (EHC) system lubricants. They are also used in some applications to lubricate steam
and gas turbines. Documents similar to D 4378 but covering phosphate ester fluids are being
developed both in ASTM and the International Standards Organization (ISO). Anzenberger
covered the program of a manufacturer of such fluids. This manufacturer provides sample
bottles in which fluid can be sent to the supplier's laboratory for testing. A report sent to
the user gives results, recommended limits, and suggested corrective action if appropriate.
Although the gas turbines covered in D 4378 are heavy duty, that is, not aircraft, the
paper by Pachuta et al. demonstrates the desirability of a monitoring program in testing
lubricants for aircraft jet engines. The methods of storing and plotting data are of interest
to any monitoring program. With increased use of aircraft derivative gas turbines for ground
applications monitoring programs for these engines can be expected in the future.
A previous symposium, "Aspects of Lubricant Oxidation," published as STP 916, dis-
cussed methods of measuring oil oxidation and the significance of oxidation on remaining
oil life. It would be well to review STP 916 in conjunction with this present document, STP
1021, since oxidation is of major concern in oil monitoring. Many of the observations of
Dr. Pachuta and his colleagues on oil oxidation, particularly those on total antioxidant
capacity (TAC), are relevant to the previous STP.
It was the intent of the symposium to review the current status of turbine oil monitoring.
It emphasized the importance of a monitoring program to maintain power generation equip-
ment in good operating condition. It is hoped that the readers of this STP will give the
editors their suggestions on improvements to D 4378 as well as their thoughts on what other
monitoring documents appropriate for power generation should be prepared under the
aUspices of D02.C.
D 4378 is the basis for an ISO document on the same subject which should be issued in
about one year. As mentioned previously, similar documents are being prepared in both
ISO and ASTM on phosphate ester fluids for electrohydraulic control (EHC) systems. As
experience accumulates with users of these documents, an appropriate subject for a future
symposium would be a review of these and user experience with them as well as an update
on D 4378.
We wish to thank the authors for their contributions, the paper reviewers for their time
and thoughts, the ASTM personnel whose efforts have resulted in this publication, and the
members of ASTM Subcomittee D02.C who prepared and reviewed D 4378.
William C. Young
General Electric, Schenectady, NY 12345;
symposium cochairman and coeditor.
Reginald S. Roberton
Princeton, NJ 08540; symposium cochair-
man and coeditor.
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Reginald S. Roberton I
Background and Development of ASTM D

4378: Practice for In-Service Monitoring
of Mineral Turbine Oils for Steam
and Gas Turbines
REFERENCE: Roberton, R. S., "Background and Development of ASTM D 4378: Practice

for In-Service Monitoring of Mineral Turbine Oils for Steam and Gas Turbines," Turbine Oil
Monitoring, ASTM STP 1021, W. C. Young and R. S. Roberton, Eds., American Society for
Testing and Materials, Philadelphia, 1989, pp. 3-18.
ABSTRACT: Several years ago a study group was set up at ASTM (American Society for
Testing and Materials) under Subcommittee C (Turbine Oils) of Committee D-2 on Petroleum
Products and Lubricants to develop a standard for in-service monitoring of steam and gas
turbine oils. The study group included well qualified and experienced representatives from
turbine equipment builders, oil producers, the power generation industry, and consultants
among its members. The objective was achieved and an ASTM standard D 4378, entitled
"Practice for In-Service Monitoring of Mineral Turbine Oils for Steam and Gas Turbines"
was issued as a single standard in 1984 and is now included in the Annual Book of ASTM
Standards. In developing the standard, it was recognized that turbine oils are unique lubricants
requiring the highest degree of oxidation stability and resistance to sludge formation and are
expected to give years of service. Also, the high cost of oil changes and unplanned shutdowns
had to be balanced against the cost of laboratory manpower and equipment for analytical
testing.
This paper covers the results of an initial study of monitoring practices within the power
generation industry and discusses in some detail why some methods in use for many years are
of doubtful significance and should be eliminated. It also describes the development of sampling
and testing schedules. To follow the oxidative degeneration of the oil, the well-established
TAN (Total Acid Number) test is retained and used in conjunction with the Rotary Bomb
Oxidation Test, (RBOT) (D 2272) 2 to provide a much more reliable indication of remaining
service life. Other properties of the oil which must be retained in service are discussed, and
major significance has also been given to the interpretation of test data and appropriate action
steps.
The technical merit of D 4378 and its acceptance by the international community is con-
firmed by the fact that it has been used by a joint working group of ISO (International Standards
Organization) and IEC (International Electrotechnical Commission) as a basis for an inter-
national maintenance and use guide.
KEY WORDS: oxidation, antioxidant, turbine severity, oxidation stability reserve, degra-
dation, oil service life, contamination, oil make up rate, warning limit
The involvement of A S T M in the preparation of an in-service monitoring practice for

turbine oils grew out of the activities of D-2 Subcommittee C, which supplements its w o r k
on standard methods with discussions on turbine oil problems and their resolution. The n e e d
Consultant, 497 Herrontown Road, Princeton, NJ 08540.

Test Method for Oxidation Stability of Steam Turbine Oils by Rotating Bomb (D 2272).
3
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4 TURBINEOIL MONITORING
for a review of lubricant test methods in use and a more systematic approach to monitoring
practices was dear. The high capital cost of equipment and the need to avoid costly unplanned
shutdowns were important considerations. As a result, a direct request was made to A S T M
by a section of the power generation industry to develop a standard monitoring practice for
steam and gas turbine oils.
In addition to the needs of utilities, both the turbine manufacturers and the major oil
producers expressed an interest in this venture. Many of the turbine builders had experienced
problems of oil degradation and difficulties associated with existing oil maintenance and
handling practices. Also, most of the major turbine oil suppliers, having for years provided
their customers with technical service, had developed some expertise in this area.
Subsequently, as a further encouragement to this effort, it became clear that the Inter-
national Standards Organization and the International Electrotechnical Commission were
becoming engaged in the preparation not only of turbine oil specifications but of an inter-
national Maintenance and Use Guide for turbine oils. This acted as a spur to complete our
work promptly so that the ASTM practice could be a possible basis for their standard.
In order to carry out this work, a new study group, Section 9, was formed in Subcommittee
C, under the chairmanship of the author, Reginald Roberton. This paper describes how the
standard was developed and highlights the areas of major significance.
Purpose and Objectives

The main purpose was to provide a monitoring practice for use by those responsible for
the operation and maintenance of power plants at major utilities and other industrial plants.
The objective was the preparation of a fairly comprehensive guide to the following:
1. An understanding of what turbine oils are, their properties, their sensitivity to con-
tamination, and how they degrade.
2. Identifying operational factors, apart from oil quality, that affect oil performance and
service life.
3. The handling of new oil deliveries and tests to run to safeguard the quality of the oil
charged to the turbines.
4. The setting up of sampling and testing schedules in order to follow changes in the oil's
condition.
5. The importance of proper sampling techniques.
6. The interpretation of test results.
7. Appropriate action steps.
Turbine Oils--Their Nature and Composition

Steam and gas turbine oils are unique lubricants. In steam turbines they must operate in
wet conditions and show exceptional stability over long periods of service. In gas turbines
they must withstand contact with very hot surfaces, often with intermittent operation and
periods of nonuse. Therefore, to be effective, both types of oil must have, in addition to
good corrosion protection and demulsibility, outstanding resistance to oxidation, which
includes a minimum tendency to form deposits in critical areas of the system.
To achieve these desired properties, it is necessary to formulate these oils from specially
refined base stocks of the highest quality plus a carefully balanced additive package. It takes
many years to develop and field test a new turbine oil formulation. The nature of these
fluids makes them very susceptible to contamination, particularly from other lubricants and
additives. A relatively small degree of contamination can markedly affect the properties and
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ROBERTON ON D 4378 5
expected service life of these lubricants. This becomes especially important at all stages of
their manufacture, transportation, and use. O n e of the objectives of the standard was to
make the user aware of the sensitive nature and application of turbine oils.
Study of Existing Practices

In commencing our work, it was felt that a good basis to start would be to m a k e a study
of test methods and practices in use in the p o w e r generation industry. With assistance from
the Edison Electric Institute ( E E I ) , who graciously allowed us to use the results of a ques-
tionnaire to utilities, and information supplied by oil producers, turbine builders, and con-
sultants, a valuable insight was obtained on industry monitoring practices. It was obvious
from the results of this study that test methods and the interpretation of test data were far
from standardized and confirmed the need for a m o r e effective and consistent approach to
monitoring oil condition.
A summary of the results of this survey are shown in Table 1. The most frequently used
tests are shown at the top of the table. It would be useful at this stage to study the relevance
of some of these tests in greater detail.
TABLE 1--Preliminary study of test methods in common use.
Test % of Users Using Test Comments
Total acid number 91 This is the most frequently run test. It is a very
valuable test, but wide variations were noted
in the controlling limits used.
Viscosity 87 Widely used. Useful but not critical. Most useful
to detect contamination.
Moisture 66 Lack of agreement on level which could be
harmful.
Color 60 Opinions vary as to significance of color. Sudden
darkening is a cause for alarm.
Sediment 45 No universal standard in use but most often
associated with cleanliness level and contam-
ination by particulate matter.
Interfacial tension 42 Still fairly widely used. Erroneously used to
detect degradation. Test is out of date since
introduction of additized oils which often have
low initial values.
Percent antioxidant 19 Considerable controversy over usefulness or
validity of this test. No recommended.
Rotary Bomb Oxidation 17 Not yet widely used but usage is growing. Shows
Test (RBOT) significant promise to follow degradation of
oil in service. Useful as a predictive tool.
Gravity 17 Often used to detect contamination.
Rust test 17 Used rarely since there is usually little change
in service if original oil is OK.
Silicon 17 Indicative of dirt contamination. Spectrographic
method not accurate or reliable.
Steam emulsion no. 11 Still used by a few power plants although no
longer an ASTM test. ASTM D 1401 demulsi-
bility is generally preferred.
Flash point 11 Only of value to detect contamination.
Oxidation by infrared 9 Used by only a few companies. Method offers
advantages over the Total Acid Number.
Water Separability 9 Accepted as a necessary requirement for new oil
(D 1401) but used very little for monitoring purposes.
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As expected, the Total Acid Number (D 974) 3 is recognized by most utilities as a useful
test for determining the oil's oxidative condition.We agree with this consensus despite the
fact that its precision is not too good at low values. Most plants have the facility for running
this test. Surprisingly, very few utilities use an infrared method for determining the oil's
condition. This may be due to lack (or cost) of equipment or to lack of a specific test method.
For many years analytical testing services laboratories and oil suppliers have used a method
based on absorption in the infrared (at 1710 cm-~). The absorbance is directly related to
the concentration of the carboxyl ( - C O O H ) functional group. As would be expected, this
also implies a correlation with Total Acid Number (TAN) results. A T A N of 0.1 is ap-
proximately equivalent to 1.0 Absorbance. The use of long (500 I~m) cells lends greater
accuracy to the IR method when applied to turbine oils. The IR method is not included in
the standard mainly because most plants do not have the equipment.
It was interesting to note the growing use of the Rotary Bomb Oxidation Test (D 2272).
In our opinion this test represents a most useful and reliable tool for determining the oxidative
state of the oil and therefore its remaining service life. The use of R B O T will be further
discussed under the section, "Quality Characteristics Which Must Be Retained In Service."
The survey also revealed the use of two tests which are unreliable and often provide
misleading information. One test is Interracial Tension (IFT) (D 971), 4 its use being based
on the assumption that oxidation of the oil is identified with the lowering of the IFT. When
the test was first used, possibly over 40 years ago, this assumption was probably correct for
the type and composition of the turbine oils on the market. A t that time new turbine oils
had very high I F T values (>40 dynes/cm), and relatively small changes in the oil's oxidative
condition resulted in a substantial drop in the IFT value. However, additive technology has
changed and now many first class turbine oils, when new, have low IFT values (around 20
dynes/cm) and do not exhibit a rapid drop in IFT when the oil starts to degrade.
The other test is the Percent Antioxidant. There is still some controversy on the subject,
but the facts are these. Historically, this is an infrared method for the determination of
DBPC (ditertiary butyl paracresol) by measuring the absorbance due to the phenolic func-
tional group. On the surface there appears to be some validity to this test if the turbine oil
antioxidant system relies entirely on DBPC. A drop in DBPC concentration is construed
as consumption (or loss) of additive and that when the concentration reaches zero the oil
would be unprotected and would degrade very quickly. However, two additional facts should
be considered. Firstly, evidence has accumulated which shows that many oils based on DBPC
have not shown marked instability when the apparent concentration of DBPC drops to zero.
Many oils have continued to give satisfactory service for years after this point. To explain
this, it has been suggested that the DBPC has entered in reactions, possibly involving trace
constituents in oil and oxygen, to form an intermediate. In this case, absorption in the
infrared due to the phenolic functional group no longer occurs, while the species retains,
to some degree, its properties as an antioxidant. Secondly, and of even more importance,
is the fact that many excellent present day turbine oils no longer rely fully or even in part
on the use of DBPC. Some oils now contain more than one antioxidant, usually of different
chemical types. It is usually possible to develop a specific test method for each antioxidant,
but this requires the knowledge of the formulation. This is outside the scope of the present
standard practice.
a Test Method for Neutralization Number by Color-Indicator Titration (D 974).

4 Test Method for Interracial Tension of Oil Against Water by the Ring Method (D 971).
Format and Contents of Standard Practice

The table of contents of the new "Practice for In-Service Monitoring of Mineral Turbine
Oils for Steam and Gas Turbines," D 4378-84a, is as follows:
Introduction
Scope
Referenced Documents
Significance and Use
Properties of Turbine Oils
Operational Factors Affecting Service Life
Sampling
Examination of New Oil on Delivery
Deterioration of Turbine Oils in Service
How Turbine Oils Degrade
Properties of Oils Which Must be Retained
Other Properties of Used Oils
Monitoring Program
Sludge and Deposits
Test Schedules
Steam Turbines
New Oil
Installation of New Oil Charge
In-Service Testing
Gas Turbines (nonaircraft derivative)
New Oil
Installation of New Oil Charge
In-Service Testing
Interpretation of Test Data and Recommended Action Steps
The following section discusses some of these topics in detail, explaining the basis for
choice of methods and concentrating on critical areas relating to oil degradation in service.
Operational Factors
In order to make the standard a self-contained guide to ensure trouble-free operation of
the turbine lubrication system, operational factors other than oil quality that affect oil service
life have been covered in some detail. These factors are:
1. Type and design of system.

2. Condition of system at startup.
3. System operating conditions.
4. Contamination.
5. Oil makeup rate.
The severity level at which a turbine operates is a combination of all the above plus
original oil quality. It is identified with the expected service life of the lubricant. The more
severe a turbine, the shorter the service life of the oil. Turbine severity has been defined as
the "Per cent of fresh oil oxidation resistance lost per year due to oil reactions in the turbine."
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An equation for calculating turbine severity is included in an Appendix to the standard.

The equation was developed by DenHerder and Vienna [1].
It is not the purpose of this paper to cover, in detail, the factors described above. This
has been done in the standard. However, the oil makeup rate deserves further comment
since it plays such a significant part in determining the life of the oil charge. In the United
States the annual makeup varies from a low of 1 to 2% to a high of 30% in extreme cases,
with an average probably around 7% per year. In turbines where makeup is low, a fairly
true picture of oil degradation is obtained based on system conditions. However, under the
same system conditions at high makeup, the oil service life will be considerably extended.
A point can be reached where makeup more or less compensates for the degree of degra-
dation and the oil has an indefinite service life. This is shown graphically in Fig. 1.
Quality Characteristics Which Must Be Retained In Service

Turbine lubrication systems are particularly sensitive to changes in oil condition, and there
should be a clear understanding by the power plant operator of what quality characteristics
of the oil are most important and how these are measured.
We have identified the following oil quality characteristics which must be retained to
ensure safe and continuous operation of the turbine: (a) viscosity; (b) oxidation stability
reserve; (c) freedom from sludge; (d) freedom from abrasive contaminants; (e) anti-corrosion
protection; (f) water separability.
These are discussed in some detail in the standard but merit further comment in view of
their importance in developing the standard.
LLI
a = ZERO H A K E - U P
._J I00. b = 15~/YR.HAKE-UP
~> c = 30S/YR.'HAKE-UP
(:3
rn
n- 75,
_J
Z
L9
n-"
o 50-
LL
0
I-- C
Z
W
r.J
25.
t.d
EL
I~0 1'2
YEARS OF SERVICE
FIG. 1--Effect of makeup on service life.
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Viscosity
Change in viscosity even by as much as plus or minus 20% would have very little effect
on lubrication. However, such an order of change usually signifies contamination, possibly
due to the use of the wrong oil as makeup. For this reason, viscosity should always be
included in a monitoring schedule. ASTM Method D 445 is normally used (ASTM Test
Method for Kinematic Viscosity of Transparent and Opaque Liquids and the Calculation
of Dynamic Viscosity).
Oxidation Stability Reserve

This is the most significant property relating to its condition and its suitability for further
service. In the development of improved high quality steam turbine oils, ASTM Method D
943, 5 known as the Turbine Oil Stability Test or TOST, has played a very significant role
despite many attempts to discredit it. Over 25 years of experience has confirmed its usefulness
and validity. In the view of our panel, it is a necessary and meaningful specification test for
new oils. Unfortunately, it is a long test (over 2000 h for a good turbine oil), making it
unsuitable for a monitoring program.
Oxidation of hydrocarbon oils proceeds by a chain mechanism initiated by a peroxide
radical. Intermediate compounds formed include aldehydes, ketones, and fatty acids. A
measure of the changes taking place can be followed in various ways, the simplest being to
monitor the change in acidity or more reliably to follow the decrease in the oxidation stability.
The acidity is measured using ASTM D 974 Total Acid Number (often called Neutalization
No.) and the oxidation stability by ASTM D 2272 Rotary Bomb Oxidation Test (RBOT).
The Total Acid Number (TAN) is easy to run but lacks precision at values between 0.1 to
0.5 mg KOH/gm, which is the range we are interested in. Therefore, we strongly advocate
that the TAN test be augmented by running the RBOT at regular intervals, particularly
when the TAN values begin to increase. Experience has shown remarkably good precision
for the RBOT on both new and used turbine oils. It has been used successfully and endorsed
by many investigators of turbine oil performance in the United States [1] and Japan [2].
The significance of actual values and trends is discussed later in this paper under "Logging
and Interpretation of Data."
Freedom from Sludge

Although for many types of lubricants this may seem a normal requirement, there is a
need to emphasize its importance with respect to steam and gas turbine oils. First, there
are many parts of turbine oil systems where even small amounts of sludge can lead to
problems and malfunction. Second, there is an unusually large amount of oil involved (up
to 7000 gal in some turbines), and, although the sludge content of the oil may be hardly
detectable, it can accumulate in sensitive areas of the system. What would be of minor
significance in other types of equipment might be catastrophic in a steam or gas turbine.
It must be borne in mind that turbine oils are highly paraffinic in nature and therefore
exhibit very poor solubility for their own oxidation products. This often leads to the phe-
nomenon of "varnishing" of metal surfaces, which occurs before the onset of visible sludge.
The oil is degraded to a point where sludge precursors are present in a quasisoluble state.
The oil should be discarded before this condition exists. Unfortunately, there are no direct
methods to measure and monitor the concentration of these sludge precursors. The condition
s Test Method for Oxidation Characteristics of Inhibited Mineral Oils (D 943).
of the oil has to be determined from its oxidation stability reserve, as measured by TAN
and RBOT.
Freedom from Abrasive Contaminants

The presence of abrasive contaminants in the oil cannot be tolerated since they promote
scoring and damage to bearings and journals as well as cause malfunction of control mech-
anisms.
The possible source of contaminants is varied. Major contamination can occur during
installation of the turbine and when it is opened for maintenance and repair. In very dusty
areas where units may be out of doors, some solids may enter through improperly installed
vents. There is also the possibility of the buildup of tramp wear metal due to wear in journal
and thrust bearings, gears, and pumps or as the result of rusting and corrosion. Possibly the
most common source is through the makeup oil when it is added to the system.
Whatever the source, these contaminants must be removed from the system by the use
of filters or centrifuge or both. In a properly maintained system with low makeup, this
presents no problem. With high makeup, careful filtration of the oil added to the turbine
is essential to minimize the risk of any possible buildup of contaminants. The oil in a well-
maintained system tends to improve in cleanliness during operation.
Cleanliness can be determined gravimetrically using ASTM F 313 (Test Method for In-
soluble Contamination of Hydraulic Fluids by Gravimetric Analysis), but the use of electronic
particle counters is becoming much more widespread. These latter instruments are good,
but in the hands of inexperienced personnel, they are subject to a wide range of errors.
Sampling is critical. Frequent standardization is required and care must be taken to ensure
that the sample contains no trace of free water, since minute water droplets are measured
as particles.
Anticorrosion Protection
Protection against rusting is very important. However, present additive technology is
extremely effective and very few turbines experience rusting problems. Antirust inhibitors
maintain their effectiveness for long periods of time, and an occasional check is all that is
necessary. ASTM Method D 665, 6 Procedure A is a satisfactory rust test for turbine oils.
Rarely is there a problem of corrosion due to acidity arising from oil oxidation since the oil
charge is removed from the system before the acidity reaches a high enough level to be
corrosive.
Water Separability--During the operation of steam turbines, separation of water from the
oil must be effective and clean. In practice this is rarely a problem since experience h a s
shown that, if the original oil charge had good demulsibility characteristics, the oil will
maintain good water separability over long periods of time. The exceptions to this are
contamination with highly emulsive oils or serious oxidative degradation. ASTM D 1401
(Test Method for Water Separability of Petroleum Oils and Synthetic Fluids) can be used
to check the oil, when necessary.
6 Test Method for Rust-Preventing Characteristics of Inhibited Mineral Oil in the Presence of Water
(D 665).
Other Properties
Although not considered an essential property, color does have some significance and
will be considered here. There is a diversity of opinion as to the significance and importance
of color degradation. In Japan many utilities include a tight color condemning limit in their
monitoring schedules, and the oil is changed merely on this basis. However, it is our ex-
perience that a gradual darkening of color is normal with many excellent fluids and is of
little concern if other tests indicate a satisfactory oil condition. On the other hand, sudden
changes in color are a warning that something is wrong and needs investigation. In this case,
if the cause is not found and remedied, accelerated oil degradation will most likely follow.
Development of the Monitoring Program

The main purpose of a monitoring program is to protect the equipment and ensure long,
trouble-free utilization of the oil in service. In general, the same type of tests can be used
for both steam and gas turbine oils, although the test frequency needs to be increased
substantially for high-severity gas turbines. The life of a turbine oil may be as long as 10 to
20 years in a steam turbine and may possibly reach or exceed 100 000 h in a low-severity
gas turbine, whereas a range of 10 000 to 30 000 h would be considered satisfactory for a
high-severity gas turbine oil. A monitoring program should not include unnecessary testing
since this is expensive, but it must ensure protection in cases of unexpected changes in
operational factors which might lead to rapid oil degradation and consequent danger to the
equipment.
The following points were considered important in choosing the test methods and deter-
mining the frequency of testing.
1. The first twelve months of operation of a steam turbine, or 4000 h for a gas turbine,
should be used to assess the severity of the turbine oil system. This period must be covered
by a sufficiently detailed testing program in order to obtain reliable information on turbine
oil performance.
2. Following this initial period, a comparatively long period should ensue when sampling
and testing can be reduced to a minimum.
3. As the oil approaches the end of its service life, increased frequency of testing is again
required in order to determine, with some precision, the point at which the oil should be
discarded.
4. A t all times unusual results in any one area suggesting either degradation or contam-
ination have to be followed up quickly with investigation and, if necessary, increased testing
to determine the cause of the problem.
The Program
The monitoring program consists essentially of three parts, all of which are of equal
importance.
1. The sampling and testing schedule.

2. Logging and interpretation Of test data.
3. Taking necessary action steps.
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No
Sampling and Testing Schedule

The tests included in the schedules (Tables 2 and 3) are run to determine the extent of
(a) contamination and/or (b) degradation. Generally we relate viscosity, appearance, water
content, and cleanliness to contamination, whereas TAN, color, and RBOT are related to
degradation. Viscosity is not included as an indicator of degradation since TAN and RBOT
are more sensitive indicators. Oils are normally changed out before any significant viscosity
increase occurs. The use of RBOT in addition to TAN is highly recommended, and these
two tests are linked in interpreting the condition of the oil.
TABLE 2--Sampling and testing schedule--steam turbine oils.
Frequency
Test First 12-Month Operation Normal Schedule
Viscosity 1 to 3 months 3 to 6 months

Total acid no. Monthly 1 to 3 months
Appearance Daily Daily
Water Monthly 1 to 3 months
Color Weekly Weekly
Rust test 6 months 1 Year
Cleanliness 1 to 3 months 1 to 3 months
RBOT 2 to 3 months 6 to 12 months
TABLE 3---Sarnpling and testing schedule--gas turbine oils.
Frequency
Test First 6-Month Operation, h Normal Schedule, h
Viscosity 500 500

Total acid no. 500 500 to 1000
Appearance 100 100
Color 200 200
Cleanliness 500 1000
RBOT 500 to 1000 1500 to 2000
Logging and Interpretation of Test Data

The importance of keeping an up-to-date record of results needs to be stressed. In addition,
graphical representation of properties which change as the oil degrades is highly recom-
mended so that any trend can be carefully watched. Possible errors in test results can often
be detected by reference to the graphs and new samples taken for check testing. This applies
particularly to the TAN test and the RBOT.
For easy reference the standard contains a table, reproduced as Table 4 in this paper,
which gives guidance on the interpretation of test results and warning limits. Most of it is
self-explanatory. However, the rationale behind the choice of certain warning limits and
data interpretation deserves further explanation.
With respect to oxidation, not all turbine oils show the same behavior mainly due to
differences in the base stocks and additive packages used. This is illustrated in Fig. 2. Oil
A shows a low TAN value for a long period, then shows a distinctive break when the TAN
value increases very quickly. Oil B, however, shows a fairly regular increase in TAN value
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreem
during the life of the oil. Comparison of the condition of the oils at the half life point would
suggest that Oil A is the better oil, which, in fact, is not so. This is one reason why regularly
scheduled testing is necessary in order that trend changes can be detected. It should be
noted that although Fig. 2 shows an oil life of around 14 years, this is not to suggest that
this is a normal or expected lifetime for steam turbine oils. Oil life is a function of many
factors, the most important being turbine severity, which can vary widely. Oils which last
for 14 years or more in one turbine may be spent in three to four years in another turbine.
Since the oxidative condition of the oil is the most important single factor is determining
if an oil is likely to throw down sludge or take off in an accelerated oxidation mode,
considerable thought has been given to establishing safe warning limits. When the T A N
value increase is in the range 0.3 to 0.4 mg K O H / g m , the oil may be at or approaching the
end of its service life. This is based on observations of oils in service and on laboratory
studies based on the D 943 Turbine Oil Stability Test. It is significant that in the D 943 test
most oils show an accelerated oxidation rate when the TAN exceeds 0.3 mg K O H / g m .
Recent studies by Stringer, Burton, and Brown at the National Research Council, Canada
[3] have confirmed this for a number of turbine oils. Therefore, when the T A N value reaches
0.3 mg K O H / g m , the operator should be aware that the oil may be in a marginal condition.
It is at this point that several steps should be taken. Testing frequency should be increased
and, if current R B O T data are not available, regular RBOT tests should be included in the
schedule. Both the TAN and RBOT should be utilized in the final analysis to determine
the point at which the oil should be changed. An RBOT of less than 25% of that of new
oil represents a danger point even if TAN values remain consistent within the 0.3 to 0.4
range.
Cleanliness level as determined by particle counting is becoming more widely used, and
some turbine manufacturers are setting limits. As already discussed, considerable care is
._.1
'n,.
I.--
t.9
hi
t..)
Z
N
~ ~, "8 1"o 1"2 14
YEARS OF SERVICE
FIG. 2--Degradation patterns of two different turbine oils.
4x
---I
c
TABLE 4---Interpretation of test data and recommended action.
z
Oil Life Ill
Steam (S) or (Running o_
Test Warning Limit Gas Turbine (G) Hours) Interpretation Action Steps I""
Total Acid No. 0.1 to 0.2 mg S Up to 20 000 h This represents above Investigate cause. Increase O
z
Increase over KOH/gm G Up to 3000 h normal deterioration. frequency of testing--compare -4
new oil Possible causes are: with RBOT data. Consult with O
.(a) system very severe; oil supplier for possible T~
(b) anti-oxidant reinhibition. fi3
depleted;
(c) wrong oil used;
(d) oil contaminated.
Total Acid No. 0.3 to 0.4 mg S, G At any time Oil at or approaching end Look for signs of increased
Increase over KOH/gm during life of service life, (c) or (d) sediment on filters and
new oil of oil charge above may apply. centrifuge. Check RBOT. If
RBOT less than 25% of
original, review status with oil
supplier and consider oil
change. Increase test
frequency if left in system.
RBOT Less than half S Up to 20 000 h Above normal Investigate cause. Increase
value on G Up to 3000 h degradation. frequency of testing.
original oil
RBOT Less than 25% of S, G At any time Together with high TAN Resample and retest. If same,
original. indicates oil at or consider oil change.
approaching end of
service life.
Water Content Exceeds 0.2% S At any time Oil contaminated. Investigate and remedy cause.
Potential water leak. Clean system by
centrifugation. If still
unsatisfactory consider oil
change or consult oil supplier.
Cleanliness Exceeds accepted S, G At any time Source of particulates may Locate and eliminate source of
limits (Note 1) be: particulates. Clean system oil
(a) make-up oil; by filtration and/or
(b) dust or ash entering centrifuging.
system;
(c) wear condition in
system.
Rust Test D665A Light fail S Up to 20 000 h (a) The system is wet and/ Investigate cause and make
or dirty. necessary maintenance and
(b) The system is not operating changes. Check Rust
maintained properly Test. Consult oil supplier
(e.g. water drainage regarding reinhibition if test
neglected, centrifuge result unchanged.
not operating.)
Rust Test D665A Light fail S, G After 20 000 h Normal additive depletion Consult oil supplier regarding
during life in wet system. reinhibition.
of oil charge
Appearance Hazy S,G At any time Oil contains water and/or Investigate cause and remedy.
solids. Filter and/or centrifuge oil.
Color Unusual and S,G At any time This is indicative of: Determine cause and rectify.
rapid (a) contamination
darkening. or
(b) excessive degradation.
Viscosity -+20% from S, G At any time (a) Oil is contaminated Determine cause. If viscosity is
original oil or low determine flash point.
viscosity. (b) Oil is severely Change oil, if necessary.
degraded. O
IgJ
ITI
Hash Point Drop 300F or S, G At any time Probably contamination. Determine cause. Check other
more com- quality parameters. Consider --I
O
pared to new oil change. z
oil. O
Z
Foam Test D892 Exceeds fol- S, G At any time Possibly contamination or Rectify cause. Check with oil
Sequence I lowing limits antifoam depletion. In supplier regarding inhibition.
Tendency---450 new turbines residual Note: Plant problems often
Stability--10 rust preventives mechanical in origin. .,4
O0
absorbed by oil may
cause problem.
..g
NOTE 1: Limits will depend on method used (consult equipment builder or oil supplier), ol
required as well as some expertise to get accurate results. Using the National Aerospace
Standard 1638 of measurement, a maximum rating of 8 is considered satisfactory, although,
in tight systems with low makeup, ratings of 6 or 7 can be obtained.
Warning limits and interpretation of other test data are more or less self explanatory.
Table 4 does include flash point and foam tests, which do not appear in the testing schedules.
These need only be used if contamination is suspected.
Taking Necessary Action Steps

Because the change in the condition of a turbine oil in service is usually very gradual,
immediate and drastic action is rarely necessary unless it is a case of contamination. There
is usually time to follow a trend and plan actions in advance. The use of the term "warning
limit" is used rather than "condemning limit" in order to alert the power plant operator
that some action is required even though the oil may still be in a usable condition. Along
with the interpretation of test data in Table 4 are recommended action steps. The interpre-
tation includes possible causes of the condition, which will assist the user to rectify the
situation. If the oil is reaching the end of its service life, this has to be confirmed. The user
is warned against taking drastic action or making important decisions based on one sample.
In the case of oxidative degradation, the use of graphical plots for TAN and R B O T are
reiterated.
The question of reinhibition often crops up. The term applies to the addition of an additive
concentrate to remedy a deficiency or loss of a certain characteristic of the system oil. For
turbine oils we consider this appropriate for reestablishing good rust protection or improving
the antifoaming qualities. In some rare cases the use of a demulsifier has proved successful.To
be effective such additions have to be carefully dispersed and the user needs to obtain the
advice and help of the oil supplier.
Reinhibition with antioxidant is not usually productive. In the author's experience, loss
of oxidation stability cannot be effectively remedied in this way. Usually the R B O T is hardly
affected by extra antioxidant, or, if an initial boost is obtained, it is not sustained. It appears
that once the oil itself has undergone substantive oxidative changes, additional inhibitor has
only a small and temporary effect. This has been substantiated by studies in actual service.
This is shown graphically in Fig. 3, which follows the R B O T of an oil in steam turbine
service, with addition of antioxidant (DBPC) at intervals. Turbine severity was rather high
in this case since the oil life was only of the order of five years. Of course, it is possible
that reinhibition may be more effective in less severe turbine service (for example, low
severity gas turbines). Should reinhibition with antioxidant be considered, it should be
reviewed with the oil supplier taking into full account the chemistry involved. Only if an
initial check shows a good RBOT response and this is maintained in service is reinhibition
likely to be beneficial.
Other Areas of Significance

Sampling
Because of its importance, sampling is covered in some detail in the standard. Poor
sampling techniques can invalidate test results and can often result in the wrong action steps
being taken. In accordance with standard D 4047 on sampling, 7 guidelines are given for
sampling from tanks, drums, lines, and reservoirs.
7 Standard Practice for Manual Sampling of Petroleum and Petroleum Products (D 4057).
4O0
Anlm~dam AntJoxidant
oI\ Added Added
,L
R 250
B
0
T \
20O
150
0
m
:73
100 0
I I I I I I I I I I I I I I I I I I I I I I I I I I I I I z
0
2 6 10 14 18 22 26 30 34 38 42 46 50 54 58 z
MONTHS OF SERVICE
FIG. 3--Effect of reinhibition with antioxidant. O~
,...t
"4
New Oil Handling

The proper handling of turbine oil during manufacture, transportation, and storage before
it is utilized has been recognized as being of fundamental importance. Turbine oils are much
more susceptible to changes in properties due to contamination than most other lubricants.
What would be considered a minor contamination for other oils could cause loss of oxidation
stability, demulsibility, and risk of deposit lay down in a turbine oil. As a result, reputable
suppliers of turbine oils take special precautions within their own manufacturing facilities
to segregate the product, usually by the use of dedicated tankage and transfer lines. Trans-
portation to the user also poses a problem and the use of dedicated road tankers and rail
cars is not always feasible, and improper cleaning procedures can lead to serious problems.
The standard gives guidance to power plant operators on the handling of new oil receipts
and for the verification of oil quality on delivery.
Conclusion
ASTM standard D 4378 is the result of detailed investigation, much discussion, and careful
reviews by many experienced personnel in all phases of the industry. It should be looked
upon as a guide and not as a strict set of test schedules. Information we have received
indicates that a number of utilities throughout the country are using it and have found it
useful to their operations. It is significant that the Joint I S O / I E C International Working
Group on Turbine Oils gladly accepted the standard as a basis for an international main-
tenance guide for turbine oils.
In the future, it is to be expected that modifications and additions will be made on the
basis of experience and need.
References
[1] Denherder, M. J. and Vienna, P. C., "Control of Turbine Oil Degradation During Use," Lubrication
Engineering, Vol. 37, No. 2, 1981, pp. 67-71.
[2] Watanabe, H. and Kobayashi, C., "Degradation of Turbine Oils---Japanese Turbine Lubrication
Practices and Problems," Lubrication Engineering, Vol. 34, No. 8, pp. 421-428.
[3] Stringer, P. L., Burton, G. E, and Brown, K. J., "Some Properties of Canadian Steam Turbine
Oils," Lubrication Engineering, Vol. 43, No. 4, 1987, pp. 283-289.
Donald Bonett I
A Turbine Lube Oil System

Monitoring Program
REFERENCE: BoneR, D., "A Turbine Lube Oil System Monitoring Program," Turbine Oil
Monitoring, ASTM STP 1021, W. C. Young and R. S. Roberton, Eds., American Society for
Testing and Materials, Philadelphia, 1989, pp. 19-24.
ABSTRACT: Con Edison has 32 steam turbines and 100 gas turbines in many locations in
New York City and Westchester County. A monitoring program is administered from a central
organization, but tested and tracked on site. The test results, when trended graphically, are
used to predict system problems and to plan corrective action with the intent to eliminate
catastrophic unit failures. The monitoring program as outlined can be used as a model to plan
a specific program.
KEY WORDS: turbines, monitoring programs, lube oil system
Historically, utilities sought the guidance and support of oil suppliers and turbine manu-
facturers for the recommendation of test and monitoring requirements for use with the
turbine lubrication system. These test requirements, methods, frequencies, and limits were
based on the system design parameters. At Consolidated Edison we modified these require-
ments to develop and implement a rigorous monitoring program that minimizes turbine
lubricant and system problems.
Basic Monitoring Program

From the 1950s through the 1970s, the Con Edison turbine lubricating oil monitoring
program consisted of weekly field tests for water content and monthly tests for neutralization
numbers. Samples were submitted to the main laboratory every three months from all turbine
reservoirs. Table 1 indicates the tests performed.
In the late 1970s the Interfacial Tension Test was discontinued and field laboratories began
to determine viscosity by using a "Visgage." The final changes were made in 1979 when we
began to concentrate our efforts on monitoring turbine lubricating oil and system cleanliness.
Samples from the main reservoir were submitted to the main laboratory at least twice per
month for particle count.
The current turbine oil monitoring program and the limits are listed in Table 2.
Con Edison has traditionally tested all deliveries of turbine lubricating oil made to the
generating stations. This is done at the main laboratory. The oil is tested and compared to
the purchase specification for ISO VG 32 (ISO V G 68 at one location) turbine grade oil.
The delivery truck is routed to our main laboratory, where the oil is sampled and tested
per the parameters listed in Table 3.
A further safeguard used to maintain turbine lubricating oil cleanliness at the generating
Senior engineer, Consolidated Edison Company of New York, New York, NY 10003.
19
Downloaded/printed
Copyright9 by
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further reproductions aut
TABLE 1--Original test program.
Viscosity
Neutralization Number
Rotating Bomb Oxidation Stability
Rust Test
Interfacial Tension
station is through the use of 5-1xm filters (absolute). The delivery truck pumps the lube oil
through the filter into the receiving tank. This maintains the integrity of the lubricating oil
and the oil system with regard to cleanliness. The filtration will reduce the particles below
Class 4 for new oil as indicated in Table 4.
Turbine lubricating oil is purchased using these stringent specifications, safeguards are
taken to assure that the specifications are met, and, finally, a monitoring program was
established and implemented.
What is done with all the data collected through the monitoring program? The first line
of defense is field testing, which is done by the station chemist. He is responsible for all
sampling and performance of the designated testing of the turbine oil. The chemist will
inform the operating personnel of all test results within the work day. If the results indicate
an out-of-limit condition, the chemist will immediately inform the operating supervisor. He
will continue to inform various levels of management at the generating station and within
the central organization. The course of corrective action to be taken is dependent on the
parameter and the level.
As an ongoing effort to predict when corrective action will be required, the chemist will
graphically track the results obtained at regular intervals. This method can be used to predict
water buildup, acid formation, viscosity changes, and any other parameter of concern. An
example of trend charts is shown in Fig. 1 (viscosity) and Fig. 2 (neutralization number).
Typical Conditions and Corrective Action

High Water--Immediate action is taken if the water level is in excess of 0.1%; the rec-
ommended action is to put all available oil conditioners in service: centrifuge and/or Bowser 2.
TABLE 2--Current test program.
Test Method Limit
Viscosity ASTM D 445~ + / - 10%

Water ASTM D 1796b 0.1% max
Neutralization number ASTM D 974' 0.3 mg/g KOH max
Rust test ASTM D 665(A)d Pass
RBOT ASTM D 2272e 100 minutes min
Particle count Electronic Class 6
" Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and the Calculation of
Dynamic Viscosity) (D 445).
h Test Method for Determination of Water and Sediment in Fuel Oils by the Centrifuge Method
(Laboratory Procedure) (D 1796).
' Test Method for Neutralization Number by Color-Indicator Titration (D 974).
d Test Method for Rust-Preventing Characteristics of Inhibited Mineral Oil in the Presence of Water
(D 665).
' Test Method for Oxidation Stability of Steam Turbine Oils by Rotating Bomb (D 2272).
-' Bowser is a manufacturer's name for an oil conditioner that has the capability to remove free water
and particles in the 40 to 100-~m (nominal) range.
,~.. , ~ ,~, ~ ~ i~:i ~ P'.I ! i
.$a,-5
I
,., ..r"
," .,J
;' ".. .2" .,.. ~
i
', *' ",, ,,,,"
......~i
9-:~.---' ! ./
b,. i 2
+J
w
O
31 ,...=-, --a z
ill
O
i J z
! i E
i O
! z
...-4
i O
.'-7:' ~ I
!i
z
1
i
i ! ! ~ ! ! i ! i i ! "u
"n
, 2 .3 ~.~ .~, 8 7 ...,= 9 I':-, !~, 1,7. -:",,.. 14- :=,.._., 18. ~,., I ~._. ~9 ~-...'~"' O
"n
FIG. 1--Viscosity trend. E
N E L I T R : A L ! - 4.,~.., ""'
' "- t,,..~;',.~ ! ' , J~U M ~'-", L'-F R TRE N D "-4
C
,-., ..~
Z
m
i o
!
r
0.Z6 .~i
E
0
0.24- z
t -I
0
z
0',2 ~ Q
i
r !g J
':?'.~,4 J # ', : 1 "
0",,i-"
.'12- I I"1 /I / 'i
/,~
I ., 1 / i / ,~
.2. / ', I II / []
0.1 l
O.,:>.~, ~ I ~' 'i ? 1 ,. i ,r
0/->6 ! I / 77
'C:'04-
. / ': !'1 iI
,,,"
':7,.02 ~. ZZ-. ..."
~__.--+ '~, ,_..
I i ! I i I ! I i I i
', 2 ,~ ,I- ,.~= 6 --r.. v= ~., ~':~', I I 12 ~,3.. i 4 1.5. ~,E 17 I ~.

t
I "=.. Z':':'
M ,7.ri'.~~
FIG. 2--Neutralization number trend.
BONETT ON MONITORING PROGRAM 23
TABLE 3---Acceptance test criteria.
Method Limit
TESTS PRIOR TO OFF LOADING

Viscosity, centistokes at 100~ ASTM D 445 28.8 to 35.2 cSt
Neut. No., mg KOH/gm of oil ASTM D 974 0.2 (max)
Steam emulsion number, s ASTM D 157-51T 200 (max)
Emulsion characteristics ASTM D 1401~ Pass
Particle count Electronic Report
Visual appearance Clear and bright
TESTS DONE THE FOLLOWINGDAY
RBOT ASTM D 2272 <200 minutes min
Rust test ASTM D 665(A) Pass
Test Method for Water Solubility of Petroleum Oils and Synthetic Fluids (D 1401).
Identify the source of the water contamination and plan for prompt repairs. If the water
content is greater than a preestablished amount, which is determined on a unit-by-unit basis
(free and/or emulsified), the unit should immediately be removed from service.
Viscosity change > + / - 1 0 % - - I f the viscosity change is < - 10%, investigate the possibility
of solvent contamination. If the viscosity change is > + 10%, this should be correlated to
the increased acidity and low RBOT 3 results, which can be indicative of product oxidation,
possibly caused by overheating.
A n increase in water level with the conditioners in service signifies a continuous leak.
Neutralization increase and viscosity increase may be due to oil degradation, oxidation taking
place, and/or hot spots in the turbine oil system. All out-of-limit parameters should be
investigated immediately.
Trending the results will target potential problem areas that will be investigated imme-
diately to prevent catastrophic failures.
Turbine lubricating oil cleanliness--monitoring and trending--The turbine lubricating oil
is sampled at least twice per month and sent to the laboratory for particle count. The oil is
passed through the oil conditioners continuously. Samples are checked before and after the
conditioners to ascertain the integrity of the conditioners. If the level of contamination
continues to increase while the conditioners are operating satisfactorily, the operators should
investigate the source of the contamination. If a large or concentrated sample of the con-
taminants can be obtained, laboratory analysis of the material will help in the investigation.
The amount of makeup oil added to the system should be tracked. This will also help in
analyzing the oil system. New oil added to the system changes the characteristics of the oil
TABLE 4---Particle count specification.
Micron Size Range,

Number of Particles per 100 mL
10-25 25-50 50-100 100-250 >250
Class 4 (new oil) 10 700 1510 225 21 0

Class 6 (in service) 42 000 6500 1000 92 0
3 ASTM Test Method for Oxidation Stability of Steam Turbine Oils by Rotating Bomb (D 2272).
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further repr
and should be noted on a trend chart. Use of the cleanliness data can determine the extent
of the flush.
In summary, testing, trending, followup, and knowledge of the turbine lubricating oil
system will avoid catastrophic turbine lubricating oil and system problems. We should not
be lulled into a false sense of security if the oil and system conditions are consistently within
limits; we should continue the established program and improve the tests, instrumentation,
and awareness.
George R. Trabert I and Gerard J. Schreuders 2
A Supplier's Approach to Turbine

Oil Monitoring
REFERENCE: Trabert, G. R. and Schreuders, G. J., "A Supplier's Approach to Turbine

Oil Monitoring," Turbine Oil Monitoring, ASTM STP 1021, W. C. Young and R. S. Roberton,
Eds., American Society for Testing and Materials, Philadelphia, 1989, pp. 25-31.
ABSTRACT: To ensure the successfuloperation of a turbine circulating oil system, the turbine
manufacturer, the turbine operator, and the lubricant supplier must cooperate by furnishing
their technical expertise.
Examples of turbine oil problems show that effective sampling procedures and monitoring
of turbine oils is required to assure a long service life. ASTM Practice for In-Service Monitoring
of Mineral Turbine Oils for Steam and Gas Turbines (D 4378) is an excellent guide to accom-
plish this.
KEY WORDS: turbine circulating oil system, turbine oil monitoring, quality control, turbine
lubricant, turbine oil analysis, warning limits, turbine oil additives
The Parties Involved

Three parties--the turbine manufacturer, the operator, and the lubricant supplier--must
work closely to ensure the successful operation of a turbine circulating oil system. Each
brings his own expertise into the process so that all aspects and details are covered. The
lubricant supplier brings expertise in petroleum handling, analytical techniques, and product
knowledge to the attention of the operator and manufacturer. Together they work to ensure
that appropriate action is taken. Figure 1 outlines the essential elements provided by each
participant to ensure long turbine oil life.
The Importance of Good Sampling

ASTM standard D 4378 [1] is a useful guide to assist those involved in the monitoring of
mineral turbine oils, and we encourage all turbine operators to use it in reviewing their
procedures.
One of the key aspects of a successful monitoring program is sampling. We would like to
add the following comments to those included in Section 6, "Sampling," of ASTM standard
D 4378.
In earlier times when economic conditions were different, oil company representatives
were often present at the time of sampling and were able to ensure that samples were
Product quality manager, Product Engineering, Chevron U.S.A. Inc., San Francisco, CA 94105-
2856.
2 Senior research engineer, Industrial Oils, Lubricants Division, Products Research Department,
Chevron Research Co., Richmond, CA 94802-0627.
25
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I Tu, ,.e ..n.ta .,rar I I Tu..,n. Opera,*, I

Design Purchasing
Manu,actur:N~ OperatingDemand:~_
QualityControl MonitoringD~k
Installation Operationand Maintenancet_~
TechnicalServic; LaboratoryFacility
-\ -\
~,JTurbine
LongOil ]I
I o,, Su..iie. I .ro.,,cfDe.,o..en,. / Life J
Blending
.u.,,oo.o/,
Oil DeliverySystem~ /
/
TechnicalServiceD/
LaboratoryAnalysis /
FIG. 1--Essential elements for long turbine oil life.
representative and not contaminated in some unusual way. Now, we usually see a sample
for the first time when it arrives at the laboratory. Therefore, it is more important than
ever that the operator obtain samples from his turbine oil system using correct procedures.
Another area of concern, particularly when systems are either filled for the first time or
drained and refilled, is to get enough samples to ensure establishing a proper baseline on
which to compare future samples. We recommend samples be taken from the following
locations:
1. From the bulk truck or drums prior to being put into customers' storage tanks.
2. From intermediate storage tanks if used.
3. From the unit itself after filling and circulation for sufficient time to ensure homo-
geneity.
It is not always necessary to analyze all the samples. If the system sample is satisfactory
and appears normal, there is no need to look at other samples. However, if the system
sample is suspect, the other samples can potentially provide a clue as to the cause.
Turbine Oil Testing: Who and What

The role of the oil supplier in the monitoring process has changed due to changing economic
conditions and product distribution processes in the oil industry. This role still varies widely
depending upon the area of the country, historic customer relationships, and market con-
ditions.
The majority of the larger utilities are doing most of the testing themselves. Some utility
companies use local independent laboratories; we recommend and support this use for timely
assistance in routine analysis of system samples. The utility testing facilities or independent
local laboratories are usually able to run several tests, such as appearance, color, total acid
number, water content, viscosity, and cleanliness. To assess remaining service life, more
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TRABERT AND SCHREUDERS ON SUPPLIER'S APPROACH 27
extensive testing is required. For example, the oxidation inhibitor content is often measured
using an infrared technique that quantifies composition in combination with an oxidation
performance test such as the Rotating Bomb Oxidation Test (RBOT), ASTM Test Method
for Oxidation Stability of Steam Turbine Oils by Rotating Bomb (D 2272). Utility or in-
dependent laboratories usually do not have the equipment or expertise to run these and
other tests of interest, such as rust prevention, wear, and metal contaminant levels.
When routine analyses begin to approach warning limits, signalling the need for more
intensive examination, or when some plant upset occurs and the oil becomes contaminated,
the oil supplier should become more actively involved in the analysis process. Most major
oil suppliers have all the laboratory equipment required to do an extensive laboratory
investigation on any turbine oil sample. Often, this equipment is utilized to provide service
to customers when an extensive analysis is required because of an actual or potential turbine
oil problem.
The amount of testing is dependent on the desire of the customer and the seriousness of
the turbine oil problem. The first test results may indicate a possible problem and more
sampling may be required to have that problem analyzed further.
Typical Turbine Circulating Oil Problems

Here are three examples of the kind of turbine circulating system problems which cus-
tomers requested the oil supplier to assist in resolving:
1. A 13 800-gal turbine oil system became contaminated with water. A centrifuge op-
eration revealed sludge as well as water. Samples of the system oil and sludge were submitted
for analysis.
2. A power plant operator complained that after a slug of water entered a turbine oil
reservoir, the oil became hazy and formed stringy, insoluble material. Oil samples from the
unit and a used-oil storage tank were received for inspection.
3. A company observed that the color of their turbine oil changed from yellow to dark
green in three months of service. A laboratory inspection of a sample of the oil was per-
formed.
TABLE 1--Analysis of system oil and centrifuge deposit from example No. 1.
Turbine Typical
Sample Source Systems New Oil Centrifuge Deposit
Oil service, Year 4 Fresh

Viscosity at 40~ cSt" 31126 29.3 ...
Viscosity at 100~ cSt" 5.31 5.13 ...
TAN, D 974, mg KOH/g 0.09 0.15
Pentane insolubles, Mass % . . . . . . 70~2
Toluene insolubles, Mass % 58.5
Water, vol % 71() <0~2 Wet
Ash, mass % 16.5
Spectroscopy analysis, <1'0 iii ...
metals, ppm"
Appearance Milky Black powder
Oxidation inhibitor, 36 100 ...
% of new oil"
" After drying sample.
TABLE 2--Analysis of oil from the unit and from the storage tank from example No. 2.
Sample Source Unit, Used Storage Tank, Used
Viscosity at 40~ cSt 33 32

TAN, D 974, mg KOH/g 0.11 0.14
Water, vol % < 0.1 0.4
Principal oxidation inhibitor 54 37
remaining, %a
Calcium, ppm 5 3
Color, D 1500 4.0 4.0
~ Approximate value based on infrared scan.
The analyses results and recommendations developed were as follows:
1. Table 1 shows the detailed analyses of the system oil and centrifuge sludge deposit.
The turbine oil analysis shows that 36% of the oxidation inhibitor remained in the oil.
Also, 7.0 vol % water was found. Other characteristics, such as viscosity and total acid
number (TAN), were normal. Wear metals were not found. Based upon these analyses, the
oil was judged to be suitable for continued service after centrifuging to remove the water.
However, close monitoring of the oil was recommended.
The centrifuge deposits were lumpy black powder. Optical microscopy identified asbestos
fibers. Spectrochemical analysis of the deposits indicated high concentrations of iron, copper,
tin, and silicon. In addition, mass spectroscopy and gas chromatography identified coal. In
summary, the centrifuge deposits consisted mainly of coal, dirt, wear metals, and asbestos
fibers. Recommendation was made to take steps to prevent excessive ingress of dirt into
the oil circulation system.
2. Inspection of the samples, the oil from the unit, and of the used oil from the oil storage
tank are listed in Table 2.
Inspection of the used oil from the unit itself shows that the oil is in good condition and
suitable for further use.
Analysis of the used oil from the storage tank shows the presence of 0.4 vol % water.
Also, the oxidation inhibitor was depleted by 63%. It was recommended to heat, centrifuge,
and filter the oil in the storage tank and then resample to ensure suitability before adding
to a turbine oil system.
3. Inspection of the "green" used turbine oil sample is listed in Table 3.
TABLE 3--Analysis of used turbine oil from example No. 3.
Sample Source Used Turbine Oil
Viscosity at 40~ cSt 30.5

Viscosity at 100~ cSt 5.2
TAN, D 974, mg KOH/g 0.11
Appearance Dark green
Filter residue, mg/100 g 12.6
Spectroscopy analysis, ppm
Aluminum 48
Iron 36
Phosphorus 26
Silicon 5
TABLE 4--Recommended warning limits for in-service steam and gas turbine oils.
ASTM Test Chevron ASTM D 4378

Oil Property Method Warning Limits Warning Limits
Appearance and odor Rapid change Hazy

Viscosity change at 40~ % max D 445 20 20
Total acid number, mg KOH/g, D 974 0.3 0.1 to 0.4 increase"
max
Water, vol %, max D 95 0.2 0.2
Calcium content, ppm, max ...h 20
Oxidation inhibitor level, % of ...' 30
new oil, min
Rust inhibitor additive content D665, Procedure A Fail test Light fail
RBOT D2272 Less than half value or
less than 25% of
original oil"
Cleanliness Exceeds accepted limitsd
Color D1500 Unusual and rapid
darkening
Flash point D 92 Drops 30~ ~ or
more compared to
new oil
Foam test, Sequence I D 892 Tendency--450 max
Stability--10 max
" Depending on oil life (running hours) and type of turbine (steam or gas).
b Atomic absorption procedure.
c Infrared procedure.
d Limits will depend on method used.
Laboratory inspection showed that the dark green oil contained a considerable a m o u n t
of sediment consisting of aluminum and lesser amounts of iron, phosphorus, and silicon
(quartz). A f t e r filtration, the oil was yellow ( A S T M D 15003 color of 2.0), typical for a used
turbine oil. The color change might be explained by the combination of the primary colors,
yellow from the turbine oil and the bluish tinge of contaminants, producing a green color.
D u e to the massive concentration of metallic residue, it was r e c o m m e n d e d to change the
oil and to d e t e r m i n e the cause of the rapid wear.
The above three examples are typical of the kind of turbine oil problems we see. T h e y
show that continuous effective monitoring of mineral turbine oils in service is r e q u i r e d to
maintain effective turbine lubrication and to assure a long service life of the turbine oil.
Turbine Oil Warning Limits

O v e r the years, our company has established warning limits for in-service steam and gas
turbine oils. W h a t is a warning limit? It's a flag that shows an oil is getting " t i r e d " but has
not reached the point where it should be " r e t i r e d . " Warning limits simply mean, " L e t ' s
watch this condition a little m o r e c a r e f u l l y - - l e t ' s sample and test the oil a little m o r e
frequently." Table 4 shows " R e c o m m e n d e d Warning Limits for In-Service Steam and Gas
Turbine Oils." N o t e the similarities with the " W a r n i n g Limits" listed in Table 3 of A S T M
D 4378 [1].
3 Test Method for ASTM Color of Petroleum Products (ASTM Color Scale) (D 1500).
Monitoring of Newly Developed Products in Turbine Oil Systems

The oil supplier is certainly involved in oil system monitoring in cases where a newly
developed turbine oil is to be field tested. A turbine oil consists of a base oil and several
types of additives. The additives usually are antioxidants, antirust agents, metal deactivators,
antifoam agents, and possibly others.
If a product reformulation takes place, for instance to improve the quality of a turbine
oil, the new product will be first extensively tested in the laboratory. If all results are
satisfactory and the new product shows customer benefits and market potential, the oil
company will proceed with a field test. Thee field test will be conducted by collecting per-
formance data from the new product in actual service in a steam or gas turbine.
Good communication with the customer is important on all details. He must be confident
that the oil supplier will make every effort, including even abortion of the test, to assure
that his operation will not suffer because of the field test. To assure the maximum value of
the test, all details must be agreed to. During the field test, the oil supplier does most of
the testing for in-service monitoring. An example of tests which are performed on a monthly
basis and additional tests done on a yearly basis is given in Table 5.
TABLE 5--List o f inspections run by an oil supplier on monthly samples taken from a gas turbine oil
development product during a field test.
9 Appearance
9 Viscosity, ASTM D 445, cSt
--40~
--100~
9 Flash point, COC, ASTM D 92, ~
9 Neutralization no., ASTM D 974
--Total acid no., mg KOH/g
9 Oxidation stability by rotating bomb, ASTM D 2272, min
9 Trace metals by spectrochemical analysis, ppm
--Silver
--Aluminum
--Boron
--Barium
--Calcium
--Cobalt
--Chromium
--Copper
--Iron
--Magnesium
--Manganese
--Molybdenum
--Sodium
--Nickel
--Phosphorus
--Lead
--Silicon
--Tin
--Titanium
--Vanadium
--Zinc
Additional tests on a yearly basis
9 Color, ASTM D 1500
9 Trace sediment, ASTM D 2273, % by vol
9 Rust-preventive test, ASTM D 665, Procedure A, 24 h
9 Oxidation inhibitor content, infrared analysis
The duration of a turbine oil field test can vary from less than a year to perhaps two
years. Occasionally, the oil company may wish to continue routine monitoring of field units
for extended periods of time. If during the field test the oil performs well in the turbine oil
system and meets the performance targets indicated by the laboratory bench test program,
the new turbine oil will probably be introduced into the marketplace.
Conclusion
Close cooperation between turbine manufacturers, turbine operators, and oil suppliers is
a very important step for good functioning of the turbine and for a long service life of the
oil.
Proper sampling of the oil in the turbine is a key to a good evaluation of the turbine oil
condition.
Monitoring of the oil in service by the A S T M D 4378 schedule and applying the required
action steps is necessary for a long trouble-free operation of turbines.
Further cooperation of the three p a r t i e s - - t h e turbine manufacturer, the operator, and
the lubricant supplier--will lead to improved ASTM procedures and A S T M test methods.
ASTM standard D 4378 has proven to be a useful vehicle, and further cooperation will lead
to refinement and improvement of this method.
Reference
[1] ASTM Practice for In-Service Monitoring of Mineral Turbine Oils for Steam and Gas Turbines (D
4378), 1987 Annual Book of ASTM Standards, ASTM Volume 05.03, Philadelphia, PA, 1987, pp.
505-518.
Ryoji Ohgake, a Motoshi Sunami, t Toshio Yoshida, 1 and
Harumichi Watanabe 1
The Reliable Control of Oil Quality in

Japanese Turbine Units
REFERENCE: Ohgake, R., Sunami, M., Yoshida, T., and Watanabe, H., "The Reliable
Control of Oil Quality in Japanese Turbine Units," Turbine Oil Monitoring, ASTM STP 1021,
W. C. Young and R. S. Roberton, Eds., American Society for Testing and Materials, Phila-
delphia, 1989, pp. 32-43.
ABSTRACT: The reliable operation of Japanese steam, gas, and water power turbines using
a newly developed trouble-resistant oil in association with a successful maintenance service
system is discussed.
A classic steam turbine oil formula containing a phenolic oxidation inhibitor and a succinic
acid-type rust inhibitor made from low-aromatic base stock has been used for trouble-free
maintenance. In Japan, the oil supplier and the user jointly administer quality control programs
for turbine oils. The accumulated data of the oil supplier are utilized for estimating the optimum
oil makeup for individual turbines. Since the installation of several computerized systems
responsible for maintaining the quality of steam turbine oil in 165 power stations, the remaining
life of the oil has been maintained over the warning limit by estimating the optimum oil's
makeup.
Remote control systems have been employed at many small hydroelectric power plants in
Japan to save manpower. Such modernization has brought about an additional lubrication
problem--severe valve sticking. More than 100 water turbine generators have suffered from
this problem since around 1965. Maintenance-free type oil was required for these units. A
new-type turbine oil for which a sludge dispersant is employed has solved this valve-sticking
problem. The evaluation method and in-service performance are provided.
The largest combined-cycle power station in the world (output 2000 MW) was recently
installed at Futsu Power Station of the Tokyo Electric Co. (in 1985). The lubrication of 14
heavy duty gas turbines (GE9001E, 113 MW) is performed by. a new high-temperature gas
turbine oil. This oil has done well, providing more than 8000 trouble-free hours of lubrication.
The oil quality monitor and control systems are discussed.
KEY WORDS: quality monitor, turbine oil, steam turbine, water turbine, gas turbine, oil
makeup, valve sticking, combined-cycle power station, lubrication and severity constant
The monitoring of turbine oil is vital for maintaining and improving the reliability of
turbine lubrication systems. Improving turbine oil formulations is important, of course, but
it is also important that the monitoring be optimal for the operating conditions of the various
types of equipment.
Steam turbines exhibit relatively m o d e r a t e oil deterioration conditions. H o w e v e r , there
is a demand for a high degree of reliability when turbines operate for long periods of time
at high capacities, which necessitates the creation of a m e t h o d for evaluating not only normal
deterioration but also unusual deterioration.
Water power turbines operate at relatively low utilization and essentially have no oil-
Nippon Oil Co., Ltd., Tokyo, Japan.
32
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OHGAKE ET AL. ON OIL QUALITY 33
cleaning equipment. Since trace amounts of sludge occurring in base stocks sometimes cause
valve sticking, dispersant type turbine oils are necessary.
Gas" turbines are exposed to rather severe conditions and sludge formation is a problem.
These conditions require the use of heat-resistant antioxidants and the establishment of an
appropriate oil-monitoring method to determine any required reconditioning and future oil
replacement.
Steam Turbines with Proper Supply Monitoring

Features of the Turbines
During the 1950s, electric power generation in Japan was almost evenly divided between
hydroelectric and thermoelectric generation. During the rapid economic growth of the 1960s,
the use of thermoelectric power increased sharply, reaching 80% of the total. In the 1980s,
nuclear power, which also uses steam turbines, came to account for 20% of the total electric
power generation.
These changes in the type of power generation were accompanied by an amazing tech-
nological revolution in the equipment used. Around 1955, the maximum capacity of one
unit at a thermoelectric power station was 66 MW; that value has now reached 1000 MW.
A t the same time, steam pressure has increased from 60 to 246 kg/cm 2, steam temperature
has risen from 480 to 566~ and oil temperature in the tank has increased by 10 to 15~
In this situation, with turbine oil being used for ten years or more, it is vital that the oil
quality be superior and that maintenance methods be established for the oil being used.
Uniform standards have not been established in Japan for these maintenance methods.
Instead, it is necessary to consider in detail the specific operating characteristics for each
piece of equipment. Fortunately, the conditions of turbine oils used in power stations are
analyzed, as a rule, every six months, and, based on these results, the remaining life of the
oil is predicted and steps taken with regard to oil makeup, replacement, etc. [1-5].
Oil Design Philosophy

Steam turbine oil is normally used for over ten years with repeated makeup. However,
during this time problems caused by oxidative degradation, sludge formation, and foam may
make it necessary to shut down the equipment. Oxidation stability is particularly important.
The Japanese quality standards restrict the total acid number to below 1.0 mg K O H / g for
the Turbine Oil Oxidation Stability (TOST) test [ASTM Test Method for Oxidation Char-
acteristics of Inhibited Mineral Oils (D 943)] equipment after 1000 h. ASTM recommends
that D 4304 (Specification for Mineral Lubricating Oil Used in Steam or Gas Turbines) the
total acid number be below 2.0 mg K O H / g after 2000 h for TOST, and that the Rotary
Bomb Oxidation Test (RBOT) life [ASTM Test Method for Oxidation Stability of Steam
Turbine Oils by Rotating Bomb (D 2272)] be under 200 min for new oil. Table 1 shows the
characteristics of typical turbine oils used in Japan. The TOST life and R B O T life are at
the high levels of over 2000 h and 200 min, respectively. In addition, it should be noted
that the amount of sludge formation after a TOST 1000 h (in accordance with A S T M D
4310 (Test Method for the Determination of the Sludging Tendencies of Inhibited Mineral
Oils) and MIL-F-17331F) is kept very low, below 10 mg.
Turbine oil is designed to meet the performance levels described above since it is used in
equipment which plays a vital role both socially and economically in supplying electricity.
For the base stocks used in turbine oils, efforts are usually made to reduce the amount of
polar compounds containing sulfur, nitrogen, aromatic compounds, etc., which tend to have
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TABLE 1--Typical properties of new turbine oils in Japan.
A B C D
Specific gravity, 15/4~ 0.8587 0.8638 0.8618 0.8637

Kinematic viscosity, mm2/s 40~ 32.43 32.05 32.02 31.65
100~ 5.607 5.458 5.555 5.402
Viscosity index 111 105 111 104
Total acid number, mg KOH/g 0.10 0.09 0.16 0.09
Color, ASTM L0.5 L0.5 L0.5 L0.5
Pour point, ~ - 12.5 -20 -20 -20
Aniline point, ~ 110.4 111.1 108.5 110.8
Refractive index, 20~ 1.4717 1.4728 1.4734 1.4726
Fraction Saturates, % 94.1 99.5 86.1 98.8
Aromatics, % 5.7 0.4 13.8 1.1
Resinous, % 0.2 0.1 0.1 0.1
Copper corrosion, 3 h at 100~ la lb 2a lb

Forming characteristics, mL (D 892) Sequence 1 20/0 <10 10/0 100/0
Sequence 2 20/0 20/0 20/0 <10
Sequence 3 10/0 <10 10/0 10/0
Air release property, min, (D 3427) 25~ 3 19.5 16.5 3.5
50~ 1 4 3.5 1
Rust preventing characteristics, D 665, pass pass pass pass
Procedure B
Oxidation stability TOST h >2000 >2000 >2000 >2000

RBOT min 230 287 200 388
Sludging tendency, mg (sludge for TOST after 3 3 6 3
IOO0h)
a negative effect on the oxidation stability of the product. This reduction is done by: (a)
solvent refining and hydrofinishing or (b) hydrocracking. Turbine oils that can endure long
use are produced from highly refined base stocks and well-balanced additive packages. The
additives used for turbine oil in Japan are combinations of phenolic antioxidants (di-tert-
butyl p-cresol, etc.) and succinic acid-type rust inhibitors. Although, to obtain longer life
oil, amine antioxidants and metallic antioxidants are also used in some cases. Care must be
taken with these additives, as incorrect use or concentration can cause sludge formation and
early discoloring of the lubricant.
The problems of foaming during actual use often appear as excessive amounts of surface
bubbles. Thus, the air release performance of the oil is important. At present, the principal
defoaming agents are nonsilicone types.
Oil Monitoring
Measurement of the oxidation life and other characteristics of turbine oil is essential for
understanding how the oil will actually perform. It is important to correctly learn the actual
environment and operating conditions for each turbine in which the oil will be used. It could
be said that by combining the characteristics of the turbines and the knowledge about the
oil used, the actual performance of turbine oil can be learned in advance. The authors'
company has more than ten years experience monitoring with computerized systems some
200 steam turbines operating in Japan. Specifically, we have introduced a turbine severity
concept defined as "severity constant" for the characterization of these turbines in the field.
Here, "severity constant" refers to the factors affecting the actual performance of the turbine
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Ag
oil, that is, the average value of decrease in the R B O T value per unit of time (4000 h)
during normal operation. For statistical purposes, 4000 h is taken to be half of a year. The
severity constant is different for each turbine; it varies widely between 5 and 30. The
distribution of the severity constant for the commercial plants monitored by Nippon Oil Co.
in Japan is shown in Fig. 1.
The number of turbines has increased from 70 to 90 since 1980. The analysis for 1980
shows that the average severity constant for all the turbines was 13.7; the value for the
current analysis, 13.4, is nearly the same. However, the distribution has widened as it used
to be centered around 5 to 15, but now there are some moderate turbines below 5 and some
very severe turbines over 20. In fact, the turbines exceeding 20 account for 14% of the total.
This change in distribution is due to the improved precision of the severity constant resulting
from an increase in the amount of monitoring data for the oil used. This range shows that
each turbine has its own individual characteristics.
The differences among equipment manufacturers and electric power companies have
decreased sharply since the 1980 analysis because of improvements in operating conditions
(the decrease of the residence time at high temperature spots, the increase of oil spray rate
to the turning gear, etc.).
The important point for optimal monitoring of each turbine (that is, for correct makeup)
is to keep a proper balance between economy and reliability. In this case, economy is
determined by deciding what level the target monitoring value should be. The margin of
safety must be determined separately for each plant. In moderate turbines, this margin is
small and favorable. However, in severe turbines, it is important that this margin be wide
enough. As a result, an appropriate method for determining the margin of safety is to use
the severity constant for each individual t u r b i n e .
Figure 2 shows an example of the oil in Turbine 2, which was used for 150 000 h at the
Y Power Station of the T Electric Power Co. The calculation for 1980 showed this turbine's
severity constant to be 10.0, the average value. T Electric Power's target monitoring value
was a RBOT value of 100 min. Adding to this value the safety margin of 10 rain obtained
from the severity constant, the appropriate supply amount for a safe target monitoring value
was obtained. As a result, the makeup required to maintain at least this value was calculated
to be about 5% for each half year. The current calculation shows the severity constant to
be 10.3, nearly the same as seven years earlier. The average supply rate per half year was
5.12%, and the turbine has been operating smoothly during this time without the target-
monitoring value ever dropping below 100 min. Makeup is performed once a year, so some
30
1980
1987
.~_ 20
10
!UUUUUUUUm-n
O 2.5 5 7.5 1O 12.5 15 17.5 20 22.5 25 27.5 30
Severity Constant
FIG. 1--D~tribution of severity constants.
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further reproductions authoriz
300 1980
estimate
250
65 200
o
m
15o
Q~
IOO
50
, , i , ~ 3 % i
o
300 1987
estimate
250
E 200
I-,- ~ ~ ~ ~ o ~
_~ 15o
lOO
50 ~ -"3%
o . . , . . . . . . \ o ~ .
0 2 4 6 8 10 12 14 16 16 20 22 24 x 104
Runninz Time, h
FIG. 2--Actual and estimated R B O T value as a function of make-up rate.
variation in the RBOT value is observed. However, during the entire seven-year period,
the value agreed almost exactly with the calculations. As a result, we can see that it is
sufficient to monitor turbines while keeping in mind a margin of safety adequate for the
intervals between makeup.
Recent P r o b l e m s with Steam Turbines

Steam turbines for commercial electric power generation have long operated at heavy
base loads, with hydroelectric power being used for load adjustment. However, with the
increase in nuclear power generation facilities, the two-shift method has been initiated for
fossil fuel thermal electric stations. With this method, some steam turbines are used for load
adjustment and operate only in the daytime when the demand for electric power is high.
As the oil load on the turbine oil increases during startup, there is a strong possibility that
the tendency toward degradation will increase. For these turbines, we analyze the data
taking into account changes in the operating mode. With nuclear power generation, a
phenomenon has been occurring that was not observed previously with steam turbines. It
had been predicted that the maximum oil temperature would be 10 to 20~ less because of
large steam turbines' supercritical pressures and that, as a result, the progress of oxidative
degradation would be extremely slow. Contrary to this prediction, however, it was discovered
that the antioxidants, which have a close connection to the life of turbine oil, were disap-
pearing. Even when the phenol antioxidants and their degradation by-products in the oil
were analyzed with gas chromatography and mass spectrometry, no difference was discovered
OHGAKE ET AL. O N OIL Q U A L I T Y 37
Number of Investigated Power Station

(145 PS)
I
I t
Trouble Free Trouble Experienced
(50PS) ( 95 PS)
I
J 1
Mechanical Trouble(35PS) Deposit TroublelOOPS)
(37% of TroubleExperienced) (03~ of TroubleExperienced)
FIG. 3--Analysis of malfunction on spool valve at water power stations.
from the case of other steam turbines, nor were any hydroperoxides detected when there
were equipment problems such as local heating.
Finding solutions to this problem will be an important task, which we are pursuing and
hope to report on in the future.
Monitoring of Water Power Turbines

Remote control systems have been employed at many small hydraulic power plants in
Japan to save manpower.
Deterioration uf Turbine Oil Deterioration of Suffer Compounds

( Oxidation of Hydrocarbons) ( Sulfur Compounds in Base Oil,
Additive, Coating Material )
RH ~ R . + - H
O.-t- 02 ~ R 0 2 " R-S-O . Oa
RO= + RH~ROOH4- O. l
'RSO, oso so,"
02
Contaminants
Organic Acid Type
Rust Inhibitor
/ oust, Wear\
~Coatin| Material)
( R'COOH) x Oust /
RCOOH
Ester Metallic Salt Sulfate

of Oroanic Acid Other Contaminants
(R~OR') (MeS04)
(RCOOMo)
Deposit
R ; Hydrocarbon
Me~Metal
FIG. 4--Valve deposit formation process.
In spite of the use of inhibited oil similar to steam turbine oil, 95 water turbine generators
have suffered from valve-sticking problems in Japan since 1965 (Fig. 3).
About 37% of the valve-sticking problems were caused by mechanical factors, but the
remaining 63% were caused by the adherence of sludge to the surface of the valves. Although
the inherent origin of this problem is the lack of oil-cleaning systems, it is judged economically
impossible to install a cleaning unit in many small hydraulic power plants.
This malfunction of the hydraulic control valves in water turbines has been a serious
problem for both the electric companies and the equipment manufacturers.
In the past it has been difficult to reproduce this phenomenon in the laboratory, so a new
test had to be devised.
Valve sticking is caused by various contaminants such as rust, coating materials, wear
particles, and deposits formed by deterioration of the oil.
The mechanism for deposit formation is believed to follow two possible major courses
(Fig. 4).
Valve deposits are composed in most cases of carboxylic acid ester metallic salt. The
sources of carboxylic acid are (a) oxidation products and deterioration of the base oil and
(b) rust preventative additives.
The next major group of the deposit is composed of metallic salt and sulfate. The sources
of sulfur are the base oil and additives. This case is noticed if, after use of straight mineral
oil for a long time, there is a change to an inhibited oil.
A laboratory testing apparatus was developed by combining a solenoid valve and a vane
pump. It has been used to effectively determine valve malfunction and valve sticking with
satisfactory repeatability.
~_va~ filter (~ ammeter
(
pu otor
y flow meter [ I
~ switch
J..
switch
solenoidvalve
FIG. 5--Laboratory testing apparatus for reproducing valve sticking.
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further reproductions author
A testing apparatus is assembled with six solenoid valves and a vane pump, which is the
same arrangement as a typical hydraulic system in a large power station (Fig. 5).
Test Method
Place 10 L of the sample oil and an appropriate amount of neat reference sludge (20 to
100 mL) into the tank.
Circulate the oil at a pressure of 20 kg/cm 2 and temperature of 60~ adjust the quantity
of oil leakage from the solenoid valves to 6 to 8 mL/min/unit in order to simulate the
quantity of leakage in an actual unit.
At this time read the ammeter and record it as the initial value.
To actuate the solenoid valve, the ammeter is increased gradually by operating the slide-
type transformer.
Thereafter, at the specified interval, actuate the solenoid valve and determine sticking
and seizure of the solenoid valve in comparison with the initial value.
Prevention of Valve Sticking

After having evaluated several types of sludge, one was selected as the reference, which
was obtained by the modification of the TOST test (ASTM D 943) using a highly refined
oil and without the presence of a copper catalyst for 500 h.
With this reference sludge, a number of additive formulations were tested. As a result,
a new "dispersant" type turbine oil has been formulated (Fig. 6) which prevents valve
sticking and has superior oxidation stability and rust preventative and antiemulsifying char-
acteristics (Table 2).
Monitoring of Gas Turbine Oil

The lubrication conditions of the General Electric large-capacity gas turbine are more
severe than those of steam turbines [6, 7]. With the temperature surrounding the bearings
over 260~ (MS7001 and 9001 model), G E has established the standard, GEK32568, re-
quiring nonvolatile antioxidants. To meet these needs, a new oil formula has been developed
specifically for gas turbines. It contains aromatic amine and a sulfur-containing hindered
phenol. This oil offers long service life and has excellent sludge prevention.
~
Sticking
~4
turbine 0il
~ 3
0 --0. <~ J7
9=-- 1
New dispersal type turbine oil
eE 0 ~ ~ ' ' ' ~J '

E
,,= 0 10 20 30 40 50 I00
Time, h
FIG. 6--Test results of valve-sticking preventative characteristics of turbine oils.
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further reproductions
40 TURBINE OIL M O N I T O R I N G
TABLE 2--Typical properties of the water turbine oils.
ASTM No. Dispersant Type Conventional
Specific gravity, 15/4~ D 1298 0.8617 0.8620

Viscosity, mmZ/s 40~ D 445 44.79 44.81
100~ 6.880 6.897
Viscosity index D 445 109 110
Total acid number, mg KOH/g D 974 0.01 0.11
Color D 1500 L0.5 L0.5
Copper corrosion, 3h at 100~ D 130 la la

Rust preventing characteristics, Procedure A D 665 pass pass
Emulsion characteristics, 54~ minutes to 3 D 1401
mL emulsion 10 3
Oxidation stability
TOST, h D 943 1600 2500
RBOT, min D 2272 220 240
Sludging tendency, mg D 4310 3 3
Valve sticking resistance ... pass fail
Performance Data for Gas Turbine Oil at Futsu Thermal Power Station o f the Tokyo
Electric Power Co., Inc.
In December 1985, the world's largest combined gas turbine cycle generator burning
liquefied natural gas (LNG) was installed at the Futsu Thermal Power Station. A combined
cycle is the use of heat recovered from exhaust of a gas turbine to help generate steam for
steam turbines at the same facility. This station consists of two groups of seven General
Electric MS9001Es for a total of 2 million KW. The station has operated satisfactorily to
date with the one group which has been in commercial operation. All units were expected
to be in full operation by November 1988.
54~ 42~
3 4
120
P
~ 100
80
60
40
nil i l, 1, n,
I i Bearing
~m Turbine 0il
FIG. 7--Outlet temperatures of turbine oil at seven bearings.
OHGAKE ET A L ON OIL QUALITY 41
~ L4
"~L3 _.-o----o- . . . . . o . . . . . . . o-. . . . . . . o
L2 ,.o- - - - ~ o'-
L1 /
o.. Make-up(5.8%)
I00 2000 o I
'i,~
I0-- . . . . (2- ~-0~ 0 Inhibitor
L ~''''"0" .... -0 . . . . . . ...~ ......... "" . . . . . "(3
8O
1 5 0 0 ~
-- 70
bo
g.
0o
/ o
~
9
9
Stage
Stage
Stage
Stage
No.1
No,2)
No.3
No.4
5O 1000
=
=
Warning
5OO
Use Limit
0 I I I
0 3 6 9 xlO3
Running Time, h
FIG. 8--Changes in operating conditions of gas turbine.
In the single-SHAFT MS9001E, the gas turbine, generator, and steam turbine are
all along the same axis and are supported by seven bearings (one on each side and one in
the center of the gas turbine; one on each side of the generator; and one on each side of
the steam turbine). The temperature of the supply oil for the gas turbine is about 55~ the
temperature of the bearing drain oil is under 70~ on each side and over 80~ in the center
(See Fig. 7).
At another temperature sensor location, the supply oil temperature of the bearing is under
40~ and the bearing drain oil temperature is only about 60~ In this case, the severity of
operation condition on the turbine oil is low.
All 14 turbines are used for the two-shift load operation.
After the turbines began operation, the oil used was sampled every 1000 to 2000 h and
its degradation checked. The following results appeared (Fig. 8):
1. The drop in the RBOT value was low: In one year (7500 h) of operation, it decreased
10% (200 min) from the initial value.
FIG. 9--1nside the bearings and the oil tank (after one year operation).
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further r
2. The residual rate of the additives was high: After one year the residual concentration
relative to new oil was 85 to 90%; this corresponded well to the rate of decrease in the
RBOT value.
3. All the parts were free of sludge: When the turbines were opened after one year,
almost no sludge was found in the oil tank or inside the bearings (Fig. 9). There was also
very little dirt in the oil filters.
4. The increase in viscosity and acid number was low, and the color increased only slightly.
Future Trends in Monitoring

At present, a regular inspection of each stage is performed once a year. (In Japan, regular
repairs, etc., at commercial power stations are performed at times determined by the Ministry
of International Trade and Industry.) However, an extension of the period of these gov-
ernment inspections closer to the two years used for steam turbines is being studied.
Since these turbines have no reserve tanks, two methods are being studied: (1) replacing
all of the turbine oil after a fixed period of continuous use (for example, once every four
years); or (2) supplying the appropriate amount of oil during the regular repairs described
above.
A t present, the compensation for each year is estimated for the supply at the scheduled
maintenance time each year, but in the future it will be necessary to select the best of the
above two methods while taking into account the degradation conditions of the oil.
Conclusion
In Japan, a classic steam turbine oil formula containing a phenolic oxidation inhibitor and
a succinic acid-type rust inhibitor made from low aromatic base stock has been used for
trouble-free maintenance by the installation of the computerized systems responsible for
maintaining the remaining life of the oil over the warning limit by estimating the optimum
oil's makeup.
A new-type turbine oil for which a sludge dispersant is employed has solved the valve-
sticking problem caused by the lack of oil cleaning systems at many small hydroelectric
power plants in Japan. Evaluation method and in-service performance are provided.
The lubrication of 14 heavy-duty gas turbines (GE9001E, 113 MW) is performed by a
new high-temperature gas turbine oil which has done well, providing more than 8000 trouble-
free hours of lubrication with a monitor system for oil quality control.
References
[1] Watanabe, H. and Kobayashi, C., "Degradation of Turbine Oils; Japanese Turbine Lubrication
Practices and Problems," Lubrication Engineering, Vol. 34, No. 8, 1978, pp. 421-428.
[2] Itabashi, S., Oba, T. and Watanabe, H., "Computerized System for Analyzing Steam Turbine Oil
in Power Stations," Lubrication Engineering, Vol. 37, No. 5, 1981, pp. 279-285.
[3] Den Herder, M. J. and Vienna, P. C., "Control of Turbine Oil Degradation During Use," Lubri-
cation Engineering, Vol. 37, No. 2, 1981, pp. 67-71.
[4] Wilson, A. C. M., "Problems Encountered with Turbine Lubricants and Associated System,"
Lubrication Engineering, Vol. 32, No. 2, 1976, pp. 60-66.
[5] Den Herder, M. J. and Bennett, H. O., "Long-life Turbine Oils for Power Generating Equipment,
ASLE preprint No. 69AM-6B-1, 1969.
[6] Den Herder, M. J., "Mineral Oil Lubrication of Large Gas Turbines," Lubrication Engineering,
Vol. 33, No. 6, 1977, pp. 303-307.
[7] Smith, A. N., "High-Temperature Lubricants for Gas Turbine Service," Lubrication Engineering,
Vol. 32, No. 2, 1976, pp. 66-69.
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further
Joseph F. Anzenberger, Sr.1
Monitoring Practices for Phosphate Ester

Fluids for Turbine Lubrication and Control
REFERENCE: Anzenberger, J. F., Sr., "Monitoring Practices for Phosphate Ester Fluids for
Turbine Lubrication and Control," Turbine Oil Monitoring, ASTM STP 1021, W. C. Young
and R. S. Roberton, Eds., American Society for Testing and Materials, Philadelphia, 1989,
pp. 44-53.
ABSTRACT: In-service monitoring of the customer's phosphate ester turbine oils has been
practiced for over 15 years. This service originated with users of electrohydraulic control (EHC)
fluids and gradually expanded to include specialty-type synthetic triaryl phosphate ester lu-
bricants for large and medium-sized gas turbines and turbine-compressor operations. In-service
monitoring is intended to assist the user in caring for the fluid to obtain maximum service life.
Users who avail themselves of this service have their used fluids examined for various prop-
erties, which could include as many as seven measurements: viscosity, acid number, specific
gravity, water content, mineral oil content, fire properties, and stability. Corrective actions
are suggested if a fluid exceeds certain property measurements.
KEY WORDS: turbine lubrication, electrohydraulic control (EHC) system, EHC fluid, Alcor
Deposition Test, fluid resistivity, phosphate ester
Fluid-related hydraulic system problems represent a potentially critical situation in the

proper control of turbine operations. The high-pressure hydraulic operations of an elec-
trohydraulic control (EHC) system consist of the hydraulic power unit, the emergency trip
system, and the steam valve control system. The nature of the system components dictates
the necessity of a high degree of cleanliness and maintenance of certain physical and chemical
properties of the EHC fluid. Because of the high pressure, the use of synthetic phosphate
ester fluid as a working medium is recommended by certain steam turbine manufacturers
to enhance the safety of operations. As a producer of approved phosphate ester fluids for
EHC systems, we have a long-standing reputation for assisting EHC fluid customers in
assessing the overall condition of their in-service fluid. This paper will review the monitoring
practices for phosphate ester fluids for turbine lubrication and control.
Discussion
Most users of phosphate ester hydraulic control fluids rely on fluid analyses to monitor
hydraulic system and component conditions. As a producer of these types of fluids, we offer
to analyze the customer's phosphate ester fluids on a periodic basis. The turbine engine
manufacturers have always recommended that regularly scheduled fluid care is needed to
ensure long, reliable operations of the hydraulic system. Hydraulic fluid analyses are intended
to supply this information,
Senior research chemist, Stauffer Chemical Co., Gallipolis Ferry, WV 25515, now retired. He lives
at 18 Mark Drive, Detmont, PA 15626.
44
Downloaded/printed
Copyright9 by
ANZENBERGER ON PHOSPHATE ESTER FLUIDS 45
TABLE 1--VACWAFS analysis coverage.
V = Viscosity, m2/s at 37.8~

A = Acid number, mg KOH/g
C = Contaminants, mineral oil, %
W = Water content, %
A = Autoignition temperature, ~
F = Foaming tendency, mL
S = Specific gravity, 60/60~
The frequency of fluid testing usually follows the original e q u i p m e n t m a n u f a c t u r e r ' s

( O E M ' s ) recommendations. W h e n we first began to offer technical service to customers, a
V A C W A F S analysis was run (Table 1) to judge the fluid's condition. Triaryl phosphate esters
are excellent solvents. It didn't take long to realize that the customers had to be supplied
with clean sampling containers that were inert to the solvent action of the fluid. Also, o t h e r
tests were soon introduced and became standards for establishing the condition of the
hydraulic fluid. Thus, the measurements in Table 2 are now m a d e with all incoming samples
of E H C fluid.
Results
Viscosity
Viscosity affects fluid flow in pipes and is important to p u m p life and system response
time. O u r experience has shown that when the fluid is out of specification it has probably
been contaminated with a mineral oil, fuel, or water. The source of the contamination should
be located and corrected. Fluid which is out of specification should be brought into speci-
fication by fluid m a k e u p as soon as possible. A scheduled maintenance down-time for change-
out in the near future should be considered.
Acid Number
As an E H C fluid is used in service, an increase in the acid n u m b e r indicates that the fluid
may be starting to deteriorate. Maintaining a low acid n u m b e r greatly extends the life
TABLE 2--Standard tests run with all EHC fluids.
Property Test Method
Viscosity, mVs, at 37.8~ ASTM D 4451

Acid number, mg KOH/g ASTM D 9742
Mineral oil content, % ASTM D 13993
Water content, % ASTM D 17444
Resistivity, G ohm-cm ASTM D 1169, 5 D 2576
Chlorine content, ppm ASTM D 808, 7 D 13178
Particle count per 100 mL SAE-A-6D
Test Method for Kinematic Viscosity of Transparent and Opaque Liquid (and the Calculation of
Dynamic Viscosity).
2 Test Method for Neutralization Number by Color-Indicator Titration.
3 Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions.
4 Test Method for Oil Separation from Lubricating Grease During Storage.
5 Test Method for Specific Resistance (Resistivity) of Electrical Insulating Liquids.
6 Test Method for D-C Resistance or Conductance of Insulating Materials.
7 Test Method for Chlorine in INew and Used Petroleum Products (Bomb Method).
8 Test Method for Chlorine in New and Used Lubricants (Sodium Alcoholate Method).
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No fur
STANDARD
[--0, --
STANDARD
0 . 5 ~ FILTER
FLUID
RESERVOIR
FULLERS'
EARTH
,r +
FIG. 1--Use o f fihers in an EHC system.
expectancy of the E H C fluid. Fuller's earth has been used for many years to neutralize
acidic components in E H C fluids. There are two schools of thought by utility station operators
concerning the use of fuller's earth. There are those who use the earth filters only when the
acid number increases. They are in the majority. The others keep the fuller's earth filters
in place all the time. My own preference is for the use of a fuller's earth filter system (Fig.
1) that is in constant use. Thus, when the acid number begins to increase you know that
you have exhausted the acid-neutralizing ability of the adsorbent so you remove the spent
cartridge and replace it with a new one and resume the use of the fuller's earth on a full-
time basis. This practice should result in keeping the E H C fluid at a low acid number and
thus prolong the life expectancy of the fluid.
Mineral Oil
Concentrations of mineral oil greater than 4% may attack the accumulator bladders and
certain other seal materials in the system and will reduce the fire resistance of the hydraulic
fluid. Concentrations below 1% are generally the result of hydrocarbon extraction from pipe
dopes, seals, and packings. When the mineral oil concentration exceeds 1%, it may indicate
contamination from an external source. Mineral oil concentrations above 2% may be in-
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No furt
soluble in the E H C fluid, resulting in a hazy mixture. If the mineral oil concentration exceeds
3%, it may jeopardize its qualification for a fluid repurchase program.
Water Content
New phosphate ester hydraulic fluid typically contains about 0.01 to 0.03 weight % water.
A water content in used fluids of 0.15% means water is entering the system from outside,
such as from a heat exchanger or an ineffective air dryer. Corrective measures should be
taken to remove the excess water and to eliminate the source of the leak. The presence of
water will result in hydrolysis, and the concentration can affect the rate of hydrolysis (Fig.
2). Fuller's earth filtration should effectively reduce the water contamination if it is in the
range of 0.1 to 0.3% water. A t higher water levels, fuller's earth will still help to reduce
the water content, but the acid number of the fluid may increase during an extended period
of filtration. Vacuum dehydration via a'portable filtration unit or complete fluid change-
out are alternatives that can be taken.
Resistivity
Fluid resistivity is measured to determine its resistance to conduct an electric current and
thus protect the valves from electrical erosion. Fuller's earth filtration will maintain electrical
resistivity at acceptable levels. If resistivity decreases, the fuller's earth should be changed
and resistivity again measured after several days exposure to the new filter's earth. If the
E H C fluid is not responsive to new fuller's earth filtration, new fluid should be added to
the system as soon as possible.
16
12
C B
50 100 150 200 250
HOURS AT 200~
F I G . 2--Stability o f phosphate esters as a function of water concentration [ASTM Test Method of

Hydrolytic Stability of Hydraulic Fluids (Beverage Bottle Method) ( D 2619)]. A = fluid containing 1.0
wt% water; B = fluid containing 0.50% water; C = fluid containing 0.03% water.
48 TURBINE OIL M O N I T O R I N G
TABLE 3--Society of Automotive Engineers, Inc. hydraulic fluid contamination study of contamination
levels, SAE, ASTM, and AIA tentative standard for hydraulic fluids (per 100 mL).
Contamination Class
Size Range, Ixm 0 1 2 3 4
5 to 10 27 000 4600 9700 24 000 32 000

10 to 25 670 1340 2680 5 360 10 700
25 to 50 93 210 380 780 1 510
50 to 100 16 28 56 110 225
>100 1 3 5 11 21
Chlorine
T h e c h l o r i n e c o n t e n t of E H C fluids is m a i n t a i n e d at u n d e r 100 p p m to g u a r d against
serious valve erosion. N e w E H C fluid usually c o n t a i n s less t h a n 35 p p m chlorine. T h e
c h l o r i n e c o n t e n t is m o n i t o r e d to e n s u r e t h a t c h l o r i n e - c o n t a i n i n g c o n t a m i n a n t s do n o t get
into the system.
A 4" x 6" card is included with two one-pint polyethylene
sample bottles plus bag, in a m a i l i n g kit which is returned
to the fluid supplier. The customer supplies the f o l l o w i n g
information.
Technical Service Laboratory
Program Information S h e e t
Company:
I IZi0C~
Station:
Address:
City, State:
Name or title:
Telephone No.
5. Unit Number
6. Unit MImufacturer
7. Sample DIte
8. Name of fluid usecl
g. Fluid makeup Date/Quantity
10.
FIG. 3--Customer information card.
ANZs163 ON PHOSPHATE ESTER I=I_UIDS 49
TABLE 4--Typical analytical technical service report sent to the customer.
TECHNICAL SERVICE REPORT
-COMPANY-
....... SAMPLE : E2631
PRODUCT : EHC
C U S T NO. : 1"295
U N I T NO. : 2
TYPE : GE
RECEIVED : 8-14-87
ANALYTICAL TEST RESULTS
TEST
VISCOSITY, SUS, I00 210.0 200-230

M I N E R A L OIL, W T % 0.30 4.0 MAX
W A T E R CONTENT, W T % 0.11 0.2 MAX
ACIDITY, m g K O H / s 0.03 0.2 MAX
C H L O R I N E CONTENT, P P M 11. 100. MAX
RESISTIVITY, G-Ohm-cm 94.0 5.0 MIN
PARTICULATE MATTER/100 ML
S I Z E (Micrometers)
5-10 9194 24000 MAX
10-25 296 5360 MAX
25-50 34 780 MAX
50-100 7 110 MAX
>100 S 11 MAX
TECHNICAL SERVICE SUPV.
All a n a l y s e s are b a s e d u p o n s a m p l e m a t e r i a l f u r n i s h e d and

t e s t e d a n d u p o n use o r a p p l i c a t i o n of s u c h m a t e r i a l as k n o w n
Particle Count
Fluid cleanliness is essential for smooth, trouble-free operation of the E H C servovalves.
All new fluid must meet the SAE-A-6D Class 3 particle count specification (Table 3). This
measurement can be made with a H I A C particle counter and uses 100 mL of fluid per test.
If the particle counts exceed these recommended limits, the filters must be checked for
correct micrometre sizes and alignment. Attention must also be given to the possibility of
dynamic seal failure, water in the system, a rupture of a fuller's earth cartridge, or contam-
ination with silica gel from the reservoir air breather.
Customer Reports
The customer is provided with two pint-size polyethylene bottles plus cap, data sheet (Fig.
3) to indicate the company, location, unit, unit manufacturer, fluid type, date sample
drawn, and running hours with fluid. The customer also receives a mailing kit with a pread-
dressed mailing label attached and a polyethylene bag into which the two pint sample bottles
are sealed. The samples are usually analyzed within four to five days after their receipt.
The analytical results are then mailed to the customer in as short a time as possible. All
analyses are recorded in a computer system, and individual sample results are printed as
shown in Table 4 and sent to the customer.
The frequency of sampling is dependent upon several conditions. A fluid that has been
in service and is performing well may be sampled only once a month or once every three
months depending upon the station manager and the condition of the fluid. A system that
starts out with a new fluid will submit samples of (1) new fluid put into sump, (2) fluid after
24, 48, and 168 h, (3) fluid monthly thereafter if all fluid properties are well within fluid
specification.
The Technical Service Laboratory Report (Table 4) shows the seven physical and chemical
properties discussed previously, the results of the properties measurements, and the rec-
ommended limits for each property. In the event one or more of these properties exceeds
the limits shown, the result is starred and a footnote added suggesting an appropriate action
to be taken. For example, should the mineral oil or water content values begin to increase,
the customer is requested to check for the potential source of leakage or contamination that
caused the increased amount of water or mineral oil. If the acid number exceeds 0.20 mg
K O H / g , the customer is advised to inspect and/or change the fuller's earth cartridges.
Likewise, should the resistivity value fall below 5 G ohm-cm, the customer is asked to change
the fuller's earth filters in the hope of increasing the resistivity value and maintaining it
above the 5 G ohm-cm minimum value. If the fluid does not respond to one or two changes
of fresh fuller's earth treatment within 24 h after a filter change, the customer can either
replace some of the in-use fluid with new E H C fluid or plan to change-out the whole system
during turbine shut down.
An increase in chlorine content usually is the result of a contaminant getting into the
system. Chlorinated solvents are usually responsible. Although a direct connection between
chlorine content and servovalve erosion has never been fully demonstrated (General
Electric), it is advisable to limit chlorine to 100 ppm in new and operating fluid.
New E H C fluid must meet the SAE-A-6D particle count specification for a Class III fluid
(Table 3). When a clean E H C system is filled with new E H C fluid which is circulated for
24 to 48 h, the refiltered fluid will frequently show a 5 to 10 ixm particle count of less than
1000. Because of the ease of contamination of the fluid, special care is exercised in handling
TABLE 5--Computer printout of the history of fluid analyses from a given customer.
CII'tP4~NYNO.
REGION,OH~ SI~ 2~, 1987
UNIT TYPE DATE VIS HINERO/.k~T~ ACIDCHL~ I~'SIST. ---P~TIIIA.~TE~TT~,/lOOml -

SUS OIL CI~TrEHT +,'Q. Pin O-ohs-c 5-LO 10-~ 25-50 50-100 )tO0
6E 1- 7-G4 219.0 0.20 0,06 O.Oi II. )!00.0 1034 lOB 12 3 2

4-1(rBq 218,0 0,20 0,05 0,03 34, )100,0 679 120 47 19 4
8-15'84 220,0 0.20 0".09 0.0i 31. )lO0.O 421 161 ,'~ 2 l
1- 7 - ~ 21%0 0,10 0,04 0,(~4 19, )tO0,O 1175 146 17 7 6
3-2%95 218,0 0,40 0,09 0,03 11, )100,0 204 122 1'2 9 3
8-19-~ 215.0 0.,,.0 0.08 0.03 26. )100.0 1185 70" 13 3 !
12-12-4~ 209,0 0,20 0,06 0.02 15, 8q,O 2625 22~ 49 II 3
4-11-86 207,0 0,I0 0,06 0,01 14, )100,0 2~.Ob 211 63 17 1
8-13-85 219,0 0,10 0,09 0,03 21, )!09,0 635 160 37 8 1
1- 7-97 ~8,0 0,20 0,05 0,01 29, )100,0 1418 10~ 34 13 2
3'-1B-97 207.0 O.lO 0.06 0.01 26. )lO0.O 1483 69 16 3 1
VENT ~ TEST SECTION SCHEMATIC
C. MAX.tEMP.
r TRANSFORMER
- | I
SPENT T.C.TUBE
COOLANT TEMP.CONTROL
COOLER
AND SUMP
COKING HEAD
WITH%" DIA.
RESISTANCE
AIR HEATEDTUBE
---H T.C.
| FILTER
AIR
COOLANT PUMP
9 _1
-I
I
I j
PRE$SURi-. . . .
GAGE . . . . . . . . . . . . . . . . . c T.ET -
FIG. 4--Schematic of Alcor deposition tester.
and drumming the E H C fluid by the manufacturer. This is also another reason why clean
sample bottles are supplied to the customer for returning used fluid samples for analysis.
Storing the test results in a computer and furnishing the customer with a computer printout
report also allows for a rapid retrieval of the history of analyses of a given fluid with each
customer. Thus, if a potential fluid problem is occurring, a print out summarizing the fluid
property measurements can be obtained with the samples from a given turbine operation
as shown in Table 5. Having the information summarized in this manner often allows for a
more rapid understanding of why the problem may occur.
Other Tests
In addition to the standard seven analyses run with each customer's fluid (Fig. 2), there
may be an occasional need to run additional tests to help a customer understand why a
problem occurs such as filter plugging, rapid rise in acid number, gel formation, a reduction
in resistivity, change in specific gravity, and an increase in chlorine, water, or mineral oil
TABLE 6--Alcor Deposition Test conditions.
Fluid volume, sump, mL 250

Fluid flow rate, mL/min 300
Fluid temperature: in 325
Out 450
Lower tube temperature, ~ (~ 288 (550)
Upper tube temperature, ~ (~ 315 to 427 (600 to 800)
Volume of air, CC/min 1000
Test time, h 24
TABLE 7--Effect of starting acid number on stability of fluid in Alcor Deposition Test.
Deposits, mg
Acid Number Test A Viscosity, A Tan Overall
of Test Fluid Time, h % mg KOH/g Filter Rod Rating
0.23 8.5 2.7 1.23 10.0 298 219.3

0.02 24 10.3 0.92 0.6 68 69.3
content. These tests may include the use of separation technology to isolate different com-
ponents, followed by the use of:
1. Metals analyses.
2. Infrared spectra.
3. Liquid chromatography.
4. Mass spectra.
5. SEM-EDAX.
6. Gas chromatography.
7. NMR spectra.
8. Other tests to understand and resolve the customers' problems.
Occasionally a customer may submit a sample of a solid or semisolid residue that was
found in a sump or in holding tanks. He wants to know what it is. This is when it becomes
necessary to revert to some of the above-mentioned tests to determine the composition of
the unknown material.
Gas Turbine Lubrication

Most of the foregoing discussion has dealt with EHC-type phosphate esters used as hy-
draulic fluids in steam turbines. Phosphate esters are also used in some large, industrial gas
turbines and in medium-sized gas turbines and turbine-compressor operations. These cus-
tomers are also invited to submit samples of their fluids for periodic inspection at certain
time intervals. Usually these fluids are examined for acid number, viscosity, specific gravity,
water content, mineral oil content, fire properties (flash point, fire point, and autoignition
temperature), and foaming tendency. Occasionally, a customer may ask for an evaluation
of the remaining life expectancy of a phosphate ester in service. Depending on fluid type,
kind of service, and history, the fluid may be examined in an oxidation-corrosion test, a
hydrolysis rate study, or in an Alcor Deposition Test. The latter test is usually used only
with the so-called synthetic triaryl phosphate esters and not with trixylyl phosphates, which
are sometimes referred to as natural phosphate esters. The fluids are also neutralized, usually
with activated alumina treatment, then filtered before being examined in any tests. In the
Alcor Deposition Test (ADT), 250 mL of fluid at 163~ (325~ is circulated at 300 mL/
rain by a high-temperature pump. Air is injected at 1000 cc/min into the fluid just prior to
entering the heater section. After leaving the heater section, the air-fluid mixture discharges
into the sump, which is cooled by air passing through a jacket surrounding the oil chamber.
The air that was injected into the test fluid leaves the reactor through a discharge tube.
Any volatile by-products formed from oxidized test fluid can be recovered in a receiver at
the end of the discharge tube. The test is run for 24 h, and the test rod is maintained at
288~ (550~ The top part of the rod can vary from 316 to 427~ (600 to 800~
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No furth
When the test is completed, the fluid is examined for changes in viscosity and acid number.
The tube deposits are weighed and classified into types such as flaky, crinkled, smooth,
sludge, and varnish. Filter deposits are also weighed. An overall rating is determined based
on the amount and type of deposits formed. The lower the rating value, the more stable
the fluid. Figure 4 shows a schematic of the Alcor Deposition Tester and Table 6 lists the
test conditions used. Table 7 shows the effect of the starting acid number of the stability of
a used fluid when examined in the A D T test. The used fluid as received had an acid number
of 0.23 mg K O H / g and failed to survive the 24-h test. By neutralizing the fluid with activated
alumina and then examining it in the A D T test, it gave a relatively low overall rating which
demonstrated excellent thermal-oxidative stability. In this case the customer was advised
to reduce the acid number of his fluid and to maintain the acid number at below 0.10 mg
KOH/g.
Conclusion
Most customers of phosphate ester fluids used in turbine lubrication and control are
dependent on the fluid supplier for guidance in determining how long the fluid should remain
in service. By monitoring critical physical and chemical properties of the fluids, the supplier
is able to offer guidance for maintaining the fluid in good condition. If the user heeds the
various warnings and suggestions offered by the supplier, he should realize a longer service
life for the fluid.
Donald G. Pachuta, 1 John A. Thich, 2 Ray W. Knipple, 3
Deborah A. Stephanic 4
Experiences with an Analytical Monitoring

Program Designed for Commercial
Flight Tests of Advanced MiI-L-23699
Turbine Fluids
REFERENCE: Pachuta, D. G., Thich, J. A., Knipple, R. W., and Stephanic, D. A., "Ex-
periences with an Analytical Monitoring Program Designed for Commercial Flight Tests of
Advanced Mil-L-23699 Turbine Fluids," Turbine Oil Monitoring, A S T M STP 1021, W. C.
Young and R. S. Roberton, Eds., American Society for Testing and Materials, Philadelphia,
1989, pp. 54-76.
ABSTRACT: Aviation turbine engine manufacturers possess different philosophies concerning

the qualification of new turbine fluids for commercial aircraft. Most require a flight test
employing a monitoring program that was designed to measure only basic fluid parameters
such as viscosity, total acid number, etc. Warning limits for changes in these parameters were
generally established from the performance characteristics of earlier generations of turbine
fluids and older engine designs which imposed less operational stress upon the fluid charge.
Recent flight test experience with a third generation Mil-L-23699 fluid suggests that revisions
to currently recognized programs and parameter limits should be made in order to properly
reflect modern engine hardware features, airline operating practices, and advanced additive
behavior. It is recommended that analytical techniques such as plasma-based atomic emission
spectrometry, size exclusion chromatography, gas chromatography, and thermal analysis be
integrated into existing flight test programs. A "two-stage" monitoring scheme consisting of
standard physical-chemical tests and these analytical techniques provided essential data about
the fluid's response to thermooxidative and operational stress. Compositional information
needed to detect and identify contaminants such as hydraulic and other foreign fluids was also
obtained. Specific examples are cited about the diagnostic abilities of this analytically oriented
monitoring program.
KEY WORDS: commercial aircraft, aviation turbine engines, oil monitoring program, Mil-
L-23699, flight test, analytical methods, thermal analysis, gas chromatography, liquid chro-
matography, spectrometry, metals, hydraulic fluid, water, contamination, deposits, thermal
oxidative degradation, additives, antioxidants
Obtaining engine manufacturer approval for a new aircraft turbine fluid is an extensive,
multistage process involving an array of physical and performance " b e n c h " test require-
ments, followed by a series of mechanical rig and engine test-stand studies. U p o n successful
completion of these stages, several engine manufacturers require and grant approval for a
Manager, Analytical Chemistry Department, Royal Lubricants Co., Inc., E. Hanover, NJ 07936.
2 Director of Operations, Royal Lubricants.
3 Consultant, Royal Lubricants.
4 Environmental analyst, Royal Lubricants.
54
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PACHUTA ET AL. ON MONITORING PROGRAM 55
flight test. Successful completion of all flight test requirements allows the new fluid to become
qualified for commercial use in the engine type(s) specified.
A flight evaluation program is independently arranged and conducted between a fluid
supplier and a cooperating airline. All program requirements such as the minimum number
of engines, hours of flight operation, engine-fluid monitoring tests, and criteria for final
approval of a new fluid are clearly established by the engine manufacturer. Detailed test
engine teardown inspections of all fluid-wetted parts by the engine manufacturer are prin-
cipally used to evaluate the new fluid's flight performance.
Engine manufacturer requirements for qualifying aircraft turbine fluids and fluid-change
guidelines for their in-service engines (see Table 1) were developed many years ago when
the predominant engine design employed labyrinth-type bearing seals which resulted in
corresponding fluid consumption rates on the order of 0.5 L/h. Since that time, carbon seal
based engine designs have become predominant, which in turn have reduced turbine fluid
consumption rates to approximately 0.02 to 0.20 L/h. This decrease in consumption rate
was soon accompanied by reductions in cycle times and operational temperature increases
in some higher thrust engines. For example, transient fluid exposure temperatures can reach
approximately 370~ in some cases. Long-standing maintenance practices of some airlines
involving no fixed fluid-change intervals have also continued. Such factors have imposed
increased thermooxidative and operational stresses upon aviation turbine fluids.
Most often the net effect of overstressing a turbine fluid can be visually observed during
engine maintenance overhauls as increased levels of sludge, varnish, lacquer, corrosion, and
coke deposits in the fluid-wetted components of the engine. Such conditions require extensive
shop time and parts-cleaning operations to correct. They can also shorten the lifetime of
expensive engine parts by preventing sufficient cooling of critical engine components, the
proper operation of carbon seals, and subsequent increases in wear rates and wear-related
damage to gears, pumps, and bearings due to circulating carbonaceous debris. In other more
visible cases of fluid stressing, flights can be delayed or inflight engine shutdowns performed
due to fluid-filter clogging.
New generations of turbine fluids have been and will continue to be required to provide
the levels of engine protection and service lifetime needed for increasingly severe operational
regimes [1]. Advances in lubricant formulations have been greatly aided by analytical meth-
ods which were developed to investigate the mechanisms of antioxidant behavior and
TABLE 1--Typical engine manufacturer program requirements and parameter limits for flight tests or
in-service monitoring of MiI-L-23699 type fluids.
Test Used Fluid Maximum Limits

Viscosity change
[mmZ/s at 37.8~ (100~ (ASTM D 445)~ +25 to +35%
Total acid number
[mg KOH/g, (ASTM D 664)b] 2.0
Foam
[mL, (ASTM D 892)c] 300
Gravimetric solids
[mg/L, 1.2 v.m paper, (FTM 3010)a] 40
" ASTM Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and the Calcu-
lation of Dynamic Viscosity).
b ASTM Test Method for Neutralization by Potentiometric Titration.
c ASTM Test Method for Foaming Characteristics of Lubricating Oils.
Federal Test Method for Solid Particle Contamination in Aircraft Turbine Engine Lubricants (Grav-
imetric Procedure).
basestock degradiation. While much of this work remains proprietary, there are literature
reports which feature some of these methods as well as the types of synergistic and degradive
mechanisms associated with Mil-L-23699 type fluids [2-6]. Many of these works and others
[7-21] have also described the application potential of various analytical methodologies to
turbine engine monitoring programs (with most involving military aircraft).
Published reports about the incorporation of analytical methods into monitoring programs
for commercial aircraft are scant. The details of many analytical methods used for such
applications are often not available, primarily because of proprietary considerations. Unlike
applications involving electrical power generating steam and gas turbines [22], there are no
currently recommended practices for performing commercial aircraft turbine engine mon-
itoring offered by ASTM, SAE, or any other professional standards organizations. Routine
monitoring of qualified in-service turbine fluids are also not currently mandated for com-
mercial aircraft by either the engine, airframe, or accessory [for example, constant speed
drive (CSD) or auxiliary power unit (APU)] vendors or any government agency.
Historically, commercial airlines have depended primarily on engine manufacturer bul-
letins which list a monitoring program and associated fluid parameter limits for both flight
tests and routine in-service operations. For flight tests involving new generations of fluids,
however, the basic physical-chemical tests that are prescribed may not provide sufficiently
detailed information about thermooxidative conditions or insure the detection of contami-
nants that could seriously degrade fluid performance and affect the flight test.
The analytical methods which were included in this program were designed to provide
information that would complement and supplement data obtained from standard physical-
chemical tests. Their most important function was to provide unique and essential chemical
information about the fluid's response to thermooxidative stress and to detect the presence
of likely contaminants.
The overall monitoring program consisted of two major stages. A listing of the tests
employed in each stage is given in Table 2. Stage II tests were performed periodically on
all monitored units or if warranted by trend-line behavior measured from Stage I tests. This
strategy minimized the number of tests routinely performed yet provided for rapid confir-
mation and follow-up actions on any atypical result. A listing of all acronyms used to describe
these analytical techniques and associated special terms used in this paper is given in the
Appendix.
Case studies were selected to illustrate some of the problems encountered during a com-
TABLE 2--Flight test monitoring program: two stage structure.

Stage I Tests Stage II Tests
Kinematic viscosity Kinematic viscosity
[at 37.8~ (100~ ASTM D 445)] [at -40~ and 200~
(ASTM O 445)]
Total acid number (ASTM D 664) Foam test (ASTM D 892)
Water content (ASTM D 1744) Specific heat (ASTM D 3947)"
]automated titration]
Size exclusion chromatography Thermal analysis
[Royal automated method] [Royal DSC method]
Trace metals and total phosphorous Capillary gas chromatography
[Royal automated ICPES method] ]Royal automated method]
Scanning electron microscopy
X-ray fluorescence spectrometry
]Royal method]
" ASTM Test Method for Specific Heat of Aircraft Turbine Lubricants by Thermal Analysis.
mercial flight evaluation of a new turbine fluid and to demonstrate some of the capabilities
of the analytical monitoring program employed. The interpretation of each featured problem
was either supported by the airline or strongly correlated to information obtained during
subsequent engine teardown inspections.
Procedure
Monitoring Program Overview
The main objectives of this analytically oriented program were to insure the safety of
engine operations and overall integrity of the flight test so that the performance capabilities
of the new fluid could be accurately evaluated. This program included all tests mandated
by the engine manufacturer as well as additional ASTM-based physical and analytical tests.
Chromatographic methods developed in-house were used to determine proprietary additive
concentrations, monitor fluid degradation patterns, and detect the presence of likely con-
taminants. A differential scanning calorimetric method was used to measure the relative
thermooxidative stability of used fluids. This parameter was considered to be critical for
assessing the effectiveness of the new fluid's antioxidant system under actual flight conditions.
An in-house developed emission spectrometric method was used to follow engine component
wear metals, likely contaminating metals, and phosphorus (which was inherent to some
additives in the formulation).
Sampling was performed by the cooperating airline according to procedures and schedules
mandated by the engine manufacturer. Throughout this study, test results and data inter-
pretation were communicated to both the cooperating airline and the engine manufacturer
for timely review.
Analytical Methods
(a) Gas Chromatography (GC). A Varian 6000 gas chromatograph equipped with an
automatic sampler, split-splitless injector, dual capillary columns, flame ionization (FID),
and nitrogen-phosphorus (NPD) selective detectors was used for all gas chromatographic
analyses of flight test samples. The columns were 30-m fused silica types (J & W Scientific)
which had a 0.32 mm ID, a 0.25-1~m film of DB-5 stationary phase, and a 350~ upper
temperature operating limit. These columns were commonly connected to the injector (via
a two-holed ferrule) and separately to the individual detectors.
Both detector signals were simultaneously displayed on a Varian 401 data station printer-
plotter. This instrumental arrangement and temperature program from 150 to 350~ provided
for selective monitoring of most major and minor nitrogen phosphorus containing additives
present in the formulation. It also presented a general high resolution view of most volatile
and thermally stable carbon hydrogen containing basestock, additive, and degradation prod-
ucts present. The method used was designed to be capable of potentially detecting low levels
of jet fuel, petroleum based hydraulic fluid, phosphate ester based aircraft hydraulic fluids,
mixtures of aircraft turbine fluids from different manufacturers, and other foreign fluids. A
major limitation of this GC method was that nonvolatile or thermally unstable chemical
components could not be detected directly.
(b) Size Exclusion Chromatography (SEC). A Waters liquid chromatograph (LC)
equipped with a Varian LC autosampler, automatic Rheodyne loop injector, Waters column
heaters, 254-nm fixed wavelength absorbance detector (UVD), and refractive index detec-
tor (RID) was used for all SEC analyses of flight test samples. Two high-resolution 30-cm,
500-,~ (Waters Ultrastyragel) SEC columns (connected in series) with a reported molecular
weight separability range o f between approximately 100 to 10 000 (relative to polystyrene

standards) were connected to a serial arrangement of the detectors. Both UVD and RID
signals were simultaneously displayed on a Waters data module. This instrumental system
(which performs separations according to effective solvated size of a molecule) was primarily
designed for the selective monitoring of most major UV absorbing additives and their UV
active degradation products. Degradative changes in the molecular weight distribution of
non-UV absorbing basestock components could be monitored by the RID. The major
advantages of SEC are that it is a rugged, reliable technique capable of rapidly separating
and detecting the presence and buildup of many nonvolatile, high molecular weight sample
components, some of which can potentially be sludge precursors. It also complements GC
data and extends the range of chemical information obtained from the sample. Another
practical advantage is that one simple and common sample preparation (dilution-filtration)
scheme is required for both GC and SEC analyses. A major disadvantage of SEC is its
inherently lower resolving power and selectivity relative to high-temperature capillary GC
techniques.
(c) Differential Scanning Calorimetry (DSC). A Dupont Model 1090B thermal analysis
system and DSC cell was used to obtain all thermograms of flight test samples. Air at 1 bar
pressure and 25 mL/min flow was used as a cell gas. Sample weights of 2.0-mg, open, flat-
bottom aluminum sample pans and 60~ heating rates from 25 to 400~ were other
essential method parameters. With this system, the temperature at which a large, sharp
exothermic signal appeared (oxidative "breakpoint" temperature) was taken as a measure
of the "total antioxidant capacity" (TAC) of the used lubricant sample. While there is no
formally accepted definition of this term, it is intended to describe the relative capability
of a lubricant to continue tolerating normal thermooxidative stress loads without losing its
ability to perform protective functions within an engine system. Based on developmental
data obtained with this DSC method, new (unused) fluid exhibited a maximum "break-
point" temperature of 320~ A "worst case" sample taken at the end of a prolonged (280
h) Coordinating Research Council (CRC) type oxidation-corrosion test (run at 190~ had
a corresponding minimum "break-point" temperature of 275~ This "worst case" sample
displayed antioxidant exhaustion behavior (that is, TAC values reached a relative minimum
prior to 280 h which coincided with enhanced viscosity and TAN slope increases, etc.). In
this manner, the analytical working range between relative maximum and minimum TAC
levels was established.
Experimental "breakpoint" temperatures for this new fluid were observed to decrease in
a generally linear manner with increasing CRC test hours. It must be emphasized, however,
that just as viscosity and TAN curves exhibit formulation-dependent behavior during CRC-
type tests for various MiI-L-23699 products, dynamic DSC curves also exhibit formulation
dependency [16]. Other investigators have also reported formulation-dependent TAC curves
when employing pressure differential scanning calorimetry (PDSC) under isothermal ana-
lytical conditions [3,4, 7, 9,15].
DSC methods have several advantages over various chromatographic methods that are
used to estimate the TAC behavior of a lubricant. A fundamental advantage of DSC is that
it provides a measure of a fluid's total resistance to massive, rapid oxidation. The antioxidant
properties of a turbine fluid are dependent upon the nature and concentration of all the
chemical components that exhibit antioxidant behavior. This includes not only the antiox-
idant additives but also secondary antioxidant species formed by in-situ thermooxidative
reactions. Often these synergistically formed antioxidants are more effective than the original
formulation additives. Because of these factors, chromatographic methods which simply
measure the remaining formulation antioxidants can provide misleading information about
a lubricant's ability to withstand continued oxidative degradation and thermal stress.
An advantage of this dynamic DSC melthod is that it is rugged, operationally simple,

reproducible (approximately 1.5~ repeatability), rapid (analysis time less than 10 rain),
and data interpretation is straight forward. One of the disadvantages inherent to apparently
all DSC methods concerning Mil-L-23699 type fluids is that the formulation dependency of
TAC curves complicates the establishment of universally applicable "warning limits" on
TAC values.
(d) Inductively Coupled Plasma Emission Spectrometry (ICPES). A ThermoJarrelt Ash
Plasma 300 sequential-scanning instrument equipped with an autosampler, air path, and
vacuum monochromators was used to monitor the levels of wear metals, potential contam-
inant metals, and total phosphorus content in all samples. A particle size dependent method
involving simple dilution of the used fluid (50 wt/wt percent sample load) with kerosene
was routinely employed. Table 3 lists the 21 elements that were monitored, which include
wear metals as well as potential contaminant metals from sources such as dirt, cement dust,
rust-inhibited or shock-strut type hydraulic fluids, and other foreign fluids.
Emission spectrometry has been applied to monitor wear metals in turbine fluids for many
years, and these applications have been well documented. Most of the application literature,
however, has involved electrode-based instrumentation, which is widely used in military
programs. Recent and apparently future trends concerning aircraft wear metal monitoring
suggest that ICPES-based instrumentation may soon become predominant for both military
and commercial applications, especially when widespread incorporation of "fine filtration"
technology [19] begins to occur in engine designs.
The advantages of the ICPES instrumental system employed in this study are its ease of
sample preparation, high sample load capability, automated operation, flexibility of ele-
mental selection, excellent sensitivity, low detection limits, and good overall reliability. The
disadvantages of the method employed are its particle size dependence and need for sample
TABLE 3--Elements, transition types, and analytical wavelengths monitored by an ICPES test method.
Element Transition Wavelength, nm
Silver Atomic 328.07

Aluminum Atomic 308.22
Barium Ionic 233.53
Boron Atomic 208.89
Cadmium Atomic 228.80
Calcium Ionic 317.93
Chromium Ionic 267.71
Copper Atomic 327.40
Iron Ionic 259.90
Magnesium Atomic 285.21
Manganese Ionic 294.92
Molybdenum Ionic 202.02
Sodium Atomic 589.59
Nickel Ionic 231.60
Phosphorus Atomic 253.57
Lead Ionic 220.35
Silicon Atomic 251.61
Tin Atomic 284.00~
Titanium Ionic 336.12
Vanadium Ionic 292.40
Zinc Atomic 213.86
" Interelement correction for Cr is required when using this wavelength.
dilution. Analysis times of approximately 5 min per sample did not pose any problems for
this study but would be a consideration for programs involving very high daily throughput.
Results and Discussion

Case I: Insuring the Integrity o f the Engine System's Fluid Charge
Case l(a) Determination o f Foreign Turbine Fluid Contamination. Most of the engines,
CSD, and A P U systems employed in this flight test had been previously operated on one
or more Mil-L-23699 formulations from other suppliers. Changeover to the new turbine
fluid typically consisted of a simple drain-flush-fill operation. Of initial interest in this study
was the completeness of fleet changeover and the amount of residual foreign turbine fluid
remaining in each unit. Both viscosity and TAN data are not capable of supplying such
critical information. In Fig. 1, curves for Engine 324 and A P U 236 demonstrate that due
to the inherently lower phosphorus content of this new fluid compared to many other
commercial turbine fluids, the presence of these other fluids could be detected via an ICPES
method. Figures 2 through 4 demonstrate that SEC-UVD, GC-NPD, and GC-FID methods
were capable of detecting and potentially identifying the intermixed foreign turbine fluid
by the differences in their additive and basestock compositions.
Quantitative data concerning fluid intermixing are difficult to obtain without a sample of
the formerly used fluid just prior to changeover, but a minimum dilution can be established
if one assumes the formerly used fluid had remaining additive concentrations that were close
Turbine Fluid C h a r g e Moniforing

Total P Levels va. Fluid H I 1 .
1.5
1.4
1.3
1.2
1.1
~,~ 1.0
0.9
,g
9c 0.8
Jl~
F 0.6
~ 0.5
0.4
0.3
0.2
0.1
0.0 I "1 I I
0 2 4
(ThousQnds)
Fluid Hrs.
D 3 2 4 Eng + 450 s o Z 3 6 APU A 461 r'ng
FIG. 1--[~ Engine 324 found to contain residual amounts of a formerly used foreign turbine fluid
(refer to Fig. 3). + Engine 450 suspected of experiencing water contamination at approximately 1802
fluid hours (refer to Fig. 6). ~ APU found to contain a significant amount of foreign turbine fluid (refer
to Fig. 2). /~ Engine 461 found to be contaminated with hydraulic fluid at 4541 fluid hours (refer to Fig.
5A).
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further r
PACHUTA ET AL. ON MON{TORING PROGRAM 61
A
GC-F}D
Profile
New Fluid
Polyot Ester Baeeatock
Components . . . . . >
L ]. . . . . . . . Areu I
Time ( m l n . ) . . . . >
GC-FID
Profile
APU 0.1 h
Sample
Polyol Ester Basestock
Antloxldant from o
Foreign Turbine
Fluid . . . . . . . . >
Area 1 I
Time (rain.). . . . >
FIG. 2--(A) Reference profile of new MiI-L-23699 turbine fluid. (B) 236 APU sample. Comparisons
with Fig. 2A (that is, Area 1) confirm the presence of a formerly used turbine fluid.
to formulation values. Based on this assumption, typical residual levels of foreign turbine
fluid were found to be between a minimum of 1 to 10% just after the initial fill of new fluid.
Throughout the course of this 15-month evaluation study (which involved a total of eight
twin-engine aircraft), engine, CSD, and A P U samples were monitored for fluid charge
integrity. ICPES and SEC data were routinely used to screen samples for possible intermixing
with foreign turbine fluids or other contaminating fluids. Use of unauthorized "make-up"
turbine fluid in some engines, APU, and CSD units was quite infrequent, but proved to be
quickly and easily detectable using this combination of analytical methods. Improper aircraft
servicing at a distant airfield by contract maintenance crews from another airline was even-
tually traced as the apparent problem source.
A
GC-NPD
Profile
New Fluid
Major
N,P Bearing
Addlfivee - - >
II .......
Tlme (mln.) . . . . >
j
B
GC-NPD
Profile
Eng. 324
116h Sample
HoP Bearing
Additives - - >
Antloxldanl From
a Foreign Turbine
Fluld . . . . . . . . . . . >
Time (mln.) . . . . >

FIG. 3--(A) Reference profile of new Mil-L-23699 turbine fluid. (B) Engine 324 after 116fluid hours.
Comparisons with Fig. 3A confirm the presence of a formerly used turbine fluid.
The presence of intermixed turbine fluids in routine commercial fleet operations is cur-
rently not a major concern and is probably not as frequent an occurrence as possibly exists
in military operations. However, problems related to turbine fluid intermixing are expected
to become of increasing concern in the future as airlines begin to convert part or all of their
fleets to advanced generations of low-coking, highly thermally stable fluids. Since the per-
formance desired from these premium-cost fluids can be degraded by intermixing with earlier
generations of turbine fluids, periodic monitoring for fluid intermixing via analytical meth-
odology may become necessary.
Another reason for possible concern about potential fluid intermixing problems is that
future engine designs employing "unducted fan" technology could require specialized types
of turbine fluids which may not be totally compatible with current MiI-L-23699 type fluids.
Other trends toward the introduction of rust-inhibited versions of MiI-L-23699 and the
development of specialized fluids for gas turbine helicopters also indicate that analytical
methods capable of diagnosing fluid intermixing may eventually be added to some routine
monitoring programs.
Case l(b) Contamination from Fire-ResistantHydraulic Fluid. On one occasion, increases
in total phosphorus levels above normal "steady state" levels and abnormal viscosity de-
creases were found in both engines of an aircraft. Examples of this behavior are illustrated
in Figs. 1 and 9 for Engine 461. Subsequent follow-up analyses by GC-FID and GC-NPD
indicated that these atypical trends were not totally due to a possible increase in fluid
consumption. Figure 5 illustrates the presence of three prominent additional peaks in the
GC profiles of samples taken from these engines. Such peaks are typical for the major
components of phosphate-based hydraulic fluids. Comparisons of retention time and relative
peak ratio data against commercial hydraulic fluid GC profiles were successful in identifying
both the manufacturer and specific type of fluid present. Confirmation of the hydraulic
fluid's identity was obtained from the cooperating airline, who reported that this specific
hydraulic fluid was used exclusively in their fleet.
The levels of hydraulic fluid contamination found in both engines indicated possible
erroneous addition during routine fluid "make-up" operations, although this fact was never
clearly established. Standard addition techniques which involved spiking known amounts of
the suspected hydraulic fluid contaminant into new turbine fluid indicated that this contam-
inant was present at a minimum of approximately 2%. This is close to a 3 to 6% level,
which would be expected from typical 1 to 2-L make-up additions to the main fluid tank.
Rather than risk the possibility of continuing to operate this aircraft with both engines
contaminated, complete drain-flush-fill operations were performed before resampling could
confirm fluid charge contamination. Subsequent engine samples did not show any further
evidence of this hydraulic fluid, which tended to eliminate any remote possibility of leakage
between the gear box and hydraulic pump system.
Case l(c) Contamination of CSD and Engine Systems with Water. A series of water
contamination problems was experienced in the test fleet during a two-month period be-
ginning in October 1986, primarily involving several CSD units (Fig. 6), with indirect evi-
dence of engine fluid contamination. This incident demonstrated how complementary data
from various program tests were sometimes required to indirectly detect and solve external
contamination problems.
The presence of water in CSD units is apparently a relatively common problem in both
commercial and military aircraft. However, apparently few commercial airlines routinely
monitor CSD units for water [24], and appropriate monitoring has just started to be more
widely implemented by the military [25]. Due to the fact that CSD units are sealed and do
not "breathe" as compared to engine systems, which are vented, external moisture, or water
contaminated, "make-up" fluid which enters a CSD system tends to remain, accumulate,
and can eventually lead to mechanical damage.
Visual detection of water-contaminated CSD fluid via sight gauge examinations cannot
reliably prevent subsequent CSD damage as they can only reveal a grossly contaminated
essentially biphase fluid system. It must be recognized that synthetic polyol esters which are
basestocks for Mil-L-23699 type turbine fluids are much more hydrophilic than petroleum
oils. Because of this property, these ester-based fluids are capable of carrying up to ap-
proximately 4000 ppm of water at 20~ [as measured by ASTM Test Method for Water in
Liquid Petroleum Products by Karl Fischer Reagent (D 1744)] before becoming visually
hazy.
A
SEC-UVD
Profile
New Fluid
Molor UV Aellvo
Additives . . . . . >
High M.W. Low Id.W.

Exelullon ~,./ ...~ Exoluslon
Limit.--> I J 9" ",~,t --->1
Tlmo (mln.) . . . . >
SEC-UVD
Profile
Eng. 481
1.4h Sample
Molor UV Aoflv,
Additives . . . . . >
Antloxldon! From o Foreign

Turbine Fluid . . . . . --->//~
High M.W. Low M.W.

Exr Ex 9
Llmlt,--> I -.J~Umlt --->1
Time (mln.) . . . . >

FIG. 4--(A) Reference profile of new MiI-L-23699 turbine fluid. (B) Engine 481 at 1.4 fluid hours
indicating low levels of a formerly used turbine fluid which contains a high molecular weight (UV active)
antioxidant. (C) Engine 469 at 105 fluid hours illustrates a normal engine-use pattern involving the in-
situ formation of oligomeric antioxidants.
C F--
SEC-UVD
Profile
Eng. 469
105h Sample
UolorUVActive
..... > /
Additives
AHIngh:~dld.anY~.;, 0lelg.o_m_e
r_l0_;
H
HighM.W. / M.W.
Low
Exclusion Exclusion
Llmlt.--> I ~./~mlt --->l
Tlmo (mln.) . . . . >
FIG. 4--Continued.
Elevated water levels can lead to partial hydrolysis of such turbine fluid basestocks.
Hydrolysis is a direct consequence of the fact that water is a reaction product of ester
synthesis from polyhydric alcohols and fatty acids. This reaction is reversible, therefore if
CSD water levels become high and are allowed to remain in the unit, hydrolysis apparently
soon follows. Contamination-induced hydrolysis is evident in Fig. 7 from the sharp TAN
increases observed in CSD 450 samples taken one month after water contamination was
first detected at 1641 fluid hours. The TAN curves for both CSD units shown in this figure
also indicate that hydrolysis reactions were relatively slow in these systems because TAN
increases were not coincident with sharp rises in water content.
An important observation made was that if CSD water levels began to exceed approxi-
mately 1000 ppm, corrosion rates (as measured from ICPES-based Mg levels) associated
with the magnesium CSD casing would soon begin to increase significantly (see Fig. 8). As
was observed with TAN response, Mg level maxima do not necessarily coincide with the
onset of water contamination. Therefore, use of Mg or TAN monitoring data can indirectly
diagnose water contamination, but only after some degree of damage has occurred.
Detection of engine contamination from water is often not as direct as are incidences
involving CSD units. Most of the contaminating water is expected to escape from the engine
during warm-up operations due to the much higher temperatures involved (that is, typical
main fluid sump temperatures are approximately 200~ and because engines are designed
to breathe as well as being mechanically vented. In one engine suspected of being contam-
inated by water at approximately 1500 fluid hours (see Fig. 6, Engine 450 example), measured
increases in engine water content were minimal, although the CSD associated with that
engine had been seriously contaminated by water at that time (see Fig. 6,450 CSD example).
A slight increase in TAN was subsequently observed for this engine (see Fig. 7, Engine 450
example), which could have indicated some fluid hydrolysis. Because of the expected rapid
venting of water, tank dilution effects and loss of some volatile free fatty acids generated,
such TAN increases would tend to be minimal and not be as pronounced as was observed
in sealed CSD systems (see Fig. 7, 450 CSD example).
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No fu
GC-NPD
Profile
Eng. 461
4541h Sample
2. 3.
H,P Bearing
Peaks 1 - 3 Additives - - >
Phosphate
Ester-
\
Time (mln.) . . . . >
GC-FID
Profile
Eng. 498
894h Sample
Polyol Ester Basntoek
2. 3. Peaks 1 - 3
Phosphate
Estero
~ m . (mln.) . . . . >
FIG. 5--(A) Engine 461 at 4541 fluid hours indicating contamination (Peaks 1 to 3) with a phosphate
ester-based hydraulic fluid. (B) Engine 498 at 894 fluid hours indicating contamination (Peaks 1 to 3)
with a phosphate-ester based hydraulic fluid.
In some cases of engine contamination by water, it is known that main fluid filter deposit
levels can shortly increase to the point of complete plugging. The cause is thought to be
due to a "steam-cleaning" effect by engine-heated water, resulting in the partial loosening
to rapid, extensive shedding of internal carbon deposits.
Significant transient increases in carbonaceous filter debris did accompany these suspected
water contamination episodes. Visual examination of these carbon deposits revealed a "rust-
Turbine Fluid Charge Monitoring

ASTM D - - 1 1 4 4 W a t e r Content vs Fluid Hrs.
2.6
2.4
2.2
2.0
1.8
E
Q,
1.6
1.4
1.2
L.I-.
eV 1.0
G
0.8
0.6
0.4
0.') +-....._+
0.0 I i I I i i i
o 1 2 3 4
Thou.andw)
uld H o u r i
a 4 5 0 CSD + 4 5 0 Eng <> 4 1 4 CSD A 7 0 3 CSD
FIG. 6--[S] CSD from Engine 450. The sampling date associated with a sharp rise in water levels at
1641 fluid hours was 11/10/86. A fluid change was performed on 1/20/87 due to excessive water con-
tamination. + Engine 450. The sampling date associated wth the slight apparent rise in engine water
levels at 1543 fluid hours was 10/31/86. ~ CSD from Engine 414. A sample taken on 10/27/86 with
1362 fluid hours contained 6800 ppm of water, was opaque, and displayed free water. The pilot reported
a "low-oil-pressure" warning light on the 10/27flight which initiated this sampling. A CSD from Engine
703. A n immediate fluid change was performed at 1653 fluid hours when 1100 ppm o f water contamination
was found.
colored" coating on some of the carbon particles. Elemental analysis by scanning electron
microscopy-X-ray fluorescence spectrometry (SEM-XRF) determined that the "rust-col-
ored" coating consisted of submicron "dustlike" material that was comprised primarily of
Fe. Phosphorus was the only other predominant element found via SEM-XRF. A more
detailed morphological analysis was not pursued.
Wear metals in the used fluid samples, especially Fe and total phosphorus levels, under-
went slight coincidental upward jumps in this engine between approximately 1500 to 2000
fluid hours during this episode (see Figs. 8 and 1, Engine 450 examples). One possible
explanation for the slight increase in phosphorus levels is that degradation products from
phosphorus-containing additives are known to be associated with stationary carbon deposits
within the engine. The weight percent of elemental phosphorus in some deposits can also
be enriched over its corresponding percent in the fluid formulation. Therefore, it is surmised
that certain incidents which cause accelerated rates of carbon deposit mobilization can be
accompanied by observed increases in total phosphorus concentrations in fluid samples.
Increases in Fe content can be caused by a number of mechanisms including corrosion and
accelerated wear rates due to circulating carbon debris.
While it cannot be positively established that either the "rust layer" or shedding was
directly or solely caused by water contamination, the fact that significant increases in water
Turbine Fluid Charge Moniforlng

ASTM D - - 6 6 ~ TAN v= Fluid Hr=.
~o0 --
4.0
Z 2.0
1.0
0.0 ~[-': -- , ~ i i
0 2 4
FThOu=mnd )
uld Houm
D 4 5 0 CSD + 450 Eng # 414 CSD A 481 s
FIG. 7--[5] CSD from Engine 450. Samples taken approximately one month after a sharp rise in water
levels was observed at 1641 fluid hours (refer to Fig. 6A) suggest the onset o f basestock hydrolysis
reactions due to entrained water. + Engine 450. The relative TAN maximum seen at 1802 fluid hours
was from a sample taken approximately one month after a maximum in engine water content was observed
(refer to Fig. 6B). 9 CSD from Engine 414. An immediate fluid change was performed at 1362 fluid
hours when 6800 ppm o f water contamination was found (refer to Fig. 6C). A Engine 461. This curve
generally represents typical TAN behavior for test fleet engines up until approximately 3800 fluid hours
when engine starter problems were encountered.
levels also occurred in the CSD units attached to these engines during the same time period
was considered to be strong circumstantial evidence, A subsequent investigation by the
cooperating airline into these incidents revealed that at a distant airfield a contract main-
tenance group from another airline had improperly transferred the new fluid from hermet-
ically sealed quart cans into a large capacity portable fluid tank. This tank was reportedly
stored outside a hanger and contained visual amounts of water contamination. Following
the correction of this improper service practice, no similar episodes were detected.
Case II: Confirmation o f the Establishment o f an Engine-Fluid "Steady-State" C o n d i t i o n

A "steady state" condition within a turbine engine's fluid system has been described as
an operational period during which the rate of antioxidant loss due to thermooxidative stress
is closely matched by the rate of antioxidant addition into the engine via "make-up" fluid
[5]. The kinetics of these processes can be studied either individually by plotting quantitative
data obtained for each antioxidant in the formulation, or collectively via TAC profiles.
Establishment of an engine-fluid "steady state" normally requires the addition of between
one to four lubricant charge, volumes of "make-up" fluid. For engines equipped with carbon
seals, this usually represents between approximately 640 to 2500 fluid hours of flight op-
eration. These calculations are based on the assumptions that a typical engine fluid system
capacity is approximately 32 L, fluid consumption is 0.05 L per hour, and that a "stirred
flow reactor" model [5] adequately describes the kinetics of antioxidant degradation in an
aircraft turbine engine. Once a stable "steady state" has been established, relative changes
in the fluid's physical and chemical properties should become minimal. If such stable con-
ditions are not observed within the calculated period of operation or if significant departures
from established "steady state" conditions occur, the presence of abnormal engine stress,
contamination, or formulation inadequacies should be investigated.
Among the elements of performance that were desired to be monitored during this flight
test was whether or not the new turbine fluid's chemical and physical properties would
exhibit normal "steady state" behavior within engines, CSD, and A P U systems of the test
fleet. Frequent sampling and inspections of fluid filters and breather pressure checks were
among the procedures used to determine this. Graphing of viscosity, TAN, and engine data
(that is, total fluid added since zero-hours-on-fluid), as well as decay curves of total phos-
phorus levels, formulation additive levels and TAC data provided detailed information which
helped to verify the establishment of a "steady state" condition. As expected, profiles of
remaining formulation antioxidant levels (which were determined via GC-NPD and not
shown for proprietary reasons) as well as TAC curves tended to be inversely associated to
the fluid's viscometric profile.
A good agreement between TAC and viscosity trendlines was considered to be an essential
indication that "steady state" conditions with respect to the overall rates of antioxidant loss
Engine Hardware Condifion Moniforing

Mg end Fe L e v e l l vs. Fluid H i s .
150
140
130
120
110
"~ 100
~ 9o
_m 8o
o
; 7o
~ 6o
~ 5o
4o
3o
2o
10
0 .it. i l l L...: L : ~ I I !
0 2 4
(Theulandl)
Fluid Hnl,
o Mg l e v e l - , - 450 CSD + Fe l e v e l s - 450 rng
FIG. 8--[] CSD 450 Mg levels. The peak Mg level at 2219 fluid hours was taken approximately two
months after a maximum in water levels was detected on 11/10/86. + Engine 450 Fe levels. The peak
Fe level at 1125 fluid hours was taken on 11/25/86. Starter shear was concurrent with the observed Fe
increase, starting at approximately 4467 fluid hours.
V i l ~ o s i t y o t 3 7 . 8 " C v l . Fluid Hrs.
50.0
1
411.0
A
46.0
A
44.0
42.0
U 40.0
tt
38.0
0
o
E 36.0
=
34.0
32.0
30.0
28.0 I I I I
2 4
housonda)
uid H o u r s
3 2 4 Eng + 4 8 9 Eng o 5 0 0 Eng A 481 s

Total Anfloxldont Copaolty vs Fluid Hr~
330
B
320
&. 310
E
g
I.-
_~ 300
0
Q.
0
P
m 290
0
(/1
280
270 i I I i
0 2 4
FTIh o u s a n d l l )
uld H o u r s
I:1 324 [ng + 4 8 9 Eng r 5 0 0 Eng A 461 Eng
FIG. 9--Legend for both Viscosity and Total Antioxidant Capacity Graphs. [] Engine 324 (new, zero-
time test engine). A scheduled engine teardown inspection was performed at 3200fluid hours. The average
fluid consumption rate was O.031 L/h. + Engine 469 (zero-time test engine). A scheduled engine teardown
inspection was performed at 3700 fluid hours The average fluid consumption rate was 0.025 L/h. 0
Engine 500 (high time test engine, with approximately 8000 h since its last shop visit). A scheduled engine
teardown inspection was performed after 3600 h on the new fluid. The average fluid consumption rate
was 0.052 L/h. A Engine 461. A foreign object damage (FOD) initiated teardown inspection was per-
formed after 4600 fluid hours. The average fluid consumption rate was 0.042 L/h.
and replenishment were being attained. Examples of typical TAC behavior for Engines 324,
469, 500, and 461, as well as their corresponding viscosity curves and average fluid con-
sumption rate data, are given in Fig. 9. Plots of corresponding phosphorus levels for Engines
324 and 461 (excluding the abberational points previously described) shown in Fig. 1 indicate
that other major additives reached their "steady state" levels at about the same time as
TAC and viscosity parameters. Phosphorus levels also tended to follow an inverse relation-
ship to viscosity data.
TAN curves for test engines, CSDs, and APUs normally showed relatively small changes
from new (unused) fluid, with maximum typical values below 1.0 mg KOH per gram.
Comparisons of the TAN curve for Engine 461, shown in Fig. 7, with the corresponding
TAC and viscosity curves for this engine, shown in Fig. 9, demonstrate that "steady states"
with respect to these three parameters were attained coincidentally.
For this flight test study, this concidental establishment of "steady states" between several
key chemical and physical parameters along with the attainment of such "steady state"
conditions within expected operational periods were found to be useful for assessing the
normalcy of fluid performance prior to obtaining confirmatory engine inspection data. In
cases where significant departures from established "steady state" conditions were observed,
either fluid contamination or consumption rate changes were subsequently diagnosed as the
cause.
Case Ili: Establishment of the Fluid's Relative Condition During

"Steady State" Operations
The absolute levels of a lubricant's additives remaining during "steady state" operations
are related to many variables. Thermooxidative and operational stress factors such as engine
temperature regimes, residence times within these regimes, consumption rates, and for-
mulation design are among the major variables influencing additive levels within these
"steady state" periods. Throughout flight test applications it is desirable to ascertain the
degree of thermooxidative stress imposed and fluid response to various stress factors. Such
information can indicate the likely "reserve" of additive protection remaining and potentially
signal the need for a precautionary fluid change if the estimated "reserves" of critical
additives become severely depleted. Basic viscosity and TAN data cannot supply such com-
positional information but can be valuable when interpreted along with appropriate analytical
data. Historically, viscosity increases of between 25 to 35% at 37.8~ (100~ have been
primarily used as "warning limits" indicative of excessive thermooxidative stress and fluid
degradation. Filter changes and fluid charge refills have normally been recommended if such
limits are exceeded. Test results from this study, however, indicate that viscosity changes
at approximately 40~ that are on the order of 35% or more do not necessarily indicate
that a serious reduction in additive "reserve" levels has occurred. For example, as shown
in Fig. 9A, Engine 461 exhibited "steady state" viscosities that were in excess of a 35%
change. Corresponding "steady state" TAN data for this engine (see Fig. 7) indicated a
maximum TAN of 0.5 mg KOH per gram, which was well below the currently used "warning
limit" of 2.0 mg KOH per gram. A subsequent tear-down inspection of Engine 461 revealed
that it did not exhibit significant amounts of sludge or carbonaceous engine deposits. This
inspection did reveal that some of the heat shielding surrounding a high-temperature-bearing
compartment had been damaged, although the time of this occurrence and its overall sig-
nificance to engine fluid properties were not known.
TAC curves for this engine shown in Fig. 9B indicated that "reserves" of between 50 to
70% above estimated minimum levels were always present. This estimation assumes that
fluid degradation mechanisms in aircraft engines are closely simulated by CRC-type oxi-
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No furthe
dation-corrosion test behavior. It also assumes that TAC decreases linearly with constant
thermooxidative stress. The levels of proprietary antioxidants and antiwear agents that were
monitored by GC-NPD, GC-FID, and ICPES (total phosphorus) also tended to support
TAC data which indicated that sufficient levels of additive protection remained in Engine
461 and all other engine fluid charges during "steady state" operations.
SEC-UVD data was also useful in estimating the relative condition of used fluids. These
profiles revealed that higher relative levels of in-situ generated oligomeric antioxidants were
present in engine fluids displaying higher viscosities. This association is demonstrated by
the SEC-UVD profiles shown in Fig. 10 for Engines 500 and 461 when both had approxi-
mately 1000 fluid hours and viscosities at 37.8~ (100~ of 32.1 and 38.7 mm2/s, respectively.
Such analytical data along with low TAN changes and results from engine inspections sup-
ported the interpretation that Engine 461 viscosity increases were predominantly associated
with synergistic reactions involving the new fluid's antioxidant package rather than from
extensive basestock degradation.
Additional engine teardown inspections performed on Engines 324,469, and 500 showed
relatively low, acceptable levels of engine sludge and deposits associated with the "steady
state" TAC and viscosity levels shown in Fig. 9. The essentially horizontal slope of the TAC
curves also appeared to indicate that the service lifetime of this fluid was not approaching
a thermooxidative stress related limit.
In another recent commercial turbine engine study where analytical methods including
PDSC were employed it was reported [21] that it is also possible to monitor relatively small
viscosity and TAN changes in modern commercial aircraft engines, yet have a highly stressed
fluid generating significant amounts of coke deposits within fluid-wetted areas. The TAC
and chromatographic data shown in that work apparently indicated that antioxidant levels
remained relatively high.
Such discrepancies indicate that much more field experience, including engine inspection
work, may be required before DSC- or PDSC-based methods for TAC determinations and
results from other analytical techniques can be fully evaluated for relevance to engine
cleanliness. Due to the complexity and diversity of engine deposit formation mechanisms
and formulation dependence of TAC data, it is unlikely that DSC-based methods alone can
ever be used to reliably predict the cleanliness of fluid-wetted hardware. A more probable
application of TAC measurements is that like established viscosity and TAN behavior,
significant changes in TAC trendlines should be useful in diagnosing certain types of ab-
normal operational changes developing within an engine. When correlations of TAC data
to existing bench test data such as the CRC test are known, TAC monitoring appears to be
useful for supplying information about the relative thermooxidative stability of a given fluid.
Case IV." Estimating the Mechanical Integrity of Fluid-Wetted Hardware

An inherent problem associated with flight tests of any new turbine fluid involves the
lack of a prior service record for characterizing normal hardware behavior in a given system.
Especially in the early phases of this study, much dependence was placed upon prior knowl-
edge of fluid performance gained from mechanical-rig and test-stand studies. However, due
to the fact that a significant number of test engines were involved, correlations of flight test
data to subsequent test engine teardown results soon developed. When applicable, a history
of prior engine teardown results was included in these correlation studies. Engine history
searches can be invaluable for distinguishing which types of hardware problems may be
engine design related from those that may be caused by flight operations or fluid formulation
limitations.
The development of reliable "hardware condition" tests that can be easily interpreted has
PACHUTAET AL. ON MONITORINGPROGRAM 73
A SEC-UVD
Profile
Eng. 5 0 0
930h
Sample
2
Vis. = 32.1 mm / s
IdalorUVActive
Higher M.W.-Ollgomerle <-- Additives
Anlloxldant Serles ---~,~
High I d . W . . / Low M.W.
Exo,-,_,on /
Limit. > ~
\ Limit--->1
Exclusion
B SEC-UVD
Profile
Eng. 461
s ~ 1055h
Sample
2
Vis. = 38.7 mm /
/ \A /~ Uolor UV Active
.ox.t. /
Higher Id.W.-Ongomerlc /
v/
= ~ II <-- Additives
High Id.W. / \ Low M.W.

Exclusion j \ Excluelon
Llmlt.-->[/~-~ \. Limit - - - > l
FIG. IO--SEC-UVD profiles of used engine fluids with similar fluid hours and consumption rates.
(A) Engine 500 at 930 fluid hours. This sample had a viscosity of 32.1 mm2/s at 37.8~C (100~ (B)
Engine 461 at 1055 fluid hours. This sample had a viscosity of 38. 7 mm2/s at 37.8~ (IO0~
historically been and continues to be the most complex and important goal of turbine fluid
monitoring. From the "fluid-centered" emphasis of this study, it was assumed that if the
new fluid was not performing its primary design functions of cooling, minimizing wear rates
due to adhesion, spalling, abrasion, corrosion, etc., that ICPES-based wear metal data or
results from other program tests designed to monitor the fluid's condition would detect most
forms of fluid-induced mechanical stress. The primary limitation of this program was that
only progressive, method-detectable hardware failure modes which would occur over a time
period longer than the unit's sampling schedule could be diagnosed in time for corrective
actions to be taken.
An example of a different type of limitation related to "hardware-condition" monitoring
that was encountered during this study involved occasional communication problems as-
sociated with sample background. For example, as shown in Fig. 7, Engine 450 exhibited
a sharp, rapid jump in Fe content from 39 to 144 ppm. A resampling from this engine
confirmed the unusually high jump and also indicated that an apparent leveling off was
taking place. No unusual vibrations or other changes in engine operating parameters were
initially reported. Further investigations revealed, however, that the engine's starter had
sheared prior to taking the first abnormal sample, which apparently accounted for the Fe
behavior. This critical information was not initially reported to appropriate airline and
laboratory personnel. Such failures to communicate essential background information can
lead to potentially costly and unnecessary fluid changes, engine replacements, and teardown
maintenance. This in turn can lead to an undermining of the reliability and importance
placed in the overall monitoring program. Therefore, besides instituting immediate resam-
pling when atypical results are obtained, a thorough and persistent inquiry into the back-
ground facts surrounding such episodes can be critical to the accurate interpretation of test
data and to taking the proper course of remedial action.
Conclusions
Several advantages of integrating advanced analytical techniques into monitoring programs
designed for commercial flight tests of new turbine fluids were clearly demonstrated. The
analytical methods featured were rapid, rugged, easily automated, and required minimal
sample preparation. Because of these factors and the strategy employed for their use, both
labor and supply costs associated with performing these methods were nominal. Relatively
high sample throughput was possible when necessary. Therefore, both economic and work
capacity considerations should not limit the incorporation of these analytical techniques into
commercial flight test applications of similar scale. These analytical methods should also be
useful in routine monitoring programs when suspected problems arise that cannot be solved
by standard physical-chemical tests.
Included in the abilities of the two-stage analytical monitoring scheme were the detection
of turbine fluid intermixing as well as contamination from water and phosphate-based hy-
draulic fluid. Thermal methods used in conjunction with chromatographic and standard
physical-chemical tests were found to be useful in determining the relative thermooxidative
stability of used fluid samples and in studies of fluid degradation mechanisms. The infor-
mation obtained from this flight test generally supported results from another recently
reported commercial monitoring study [21] which highlighted some of the limitations of
established engine manufacturer programs and possible problems associated with currently
recognized "warning limits" for initiating costly turbine fluid changes.
Additional basic research, method development work, and correlation studies are required
in order to further improve the diagnostic capabilities of turbine fluid monitoring programs.
Continued advances in this field are important because existing "on-line" condition sensors
(that is, chip detectors) and "off-line" laboratory-based techniques still possess limited
abilities with respect to providing reliable, predictive information about the cleanliness and
state of fluid-wetted hardware within an aircraft turbine engine.
Appendix
Alphabetical Listing of Acronyms Employed
APU Auxiliary power unit
CSD Constant speed drive
CRC Coordinating Research Council
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No fu
DSC Differential scanning calorimetry

FID Flame ionization detector
FOD Foreign object damage
GC Gas chromatography
GC-FID Gas chromatography with a flame ionization detector
GC-NPD Gas chromatography with a nitrogen phosphorus selective detector
ICPES Inductively coupled plasma emission spectrometry
JOAP Joint oil analysis program
LC Liquid chromatography
NOAP Naval oil analysis program
NPD Nitrogen phosphorus selective detector
PDSC Pressurized differential scanning calorimetry
RID Refractive index detector
SEC Size exclusion chromatography
SEC-UVD Size exclusion chromatography with an ultraviolet absorbance detector
SEM-XRF Scanning electron microscopy with an X-ray fluorescence detector
TAC Total antioxidant capacity
UV Ultraviolet
UVD Ultraviolet at~sorbance detector
References
[1] Bishop, G. J., Journal of Synthetic Lubrication, 1987, Vol. 4, No. 1, p. 25.
[2] Jensen, R. K., et al., Journal of Synthetic Lubrication, 1984, Vol. 1, No. 2, p. 91.
[3] Zeman, A., et al., Journal of Synthetic Lubrication, 1985, Vol. 2, No. 2, p. 2.
[4] Zeman, A., et al., Journal of Synthetic Lubrication, 1986, Vol. 3, No. 4, p. 309
[5] Sniegoski, P. J., Lubrication Engineering, Vol. 41, No. 1, 1985, p. 11.
[6] Maier, K., Journal of Synthetic Lubrication, Vol. 3, No. 3, 1986, p. 163.
[7] Zeman, A., Schmiertechnik and Tribologie, Vol. 29, 1982, p. 55.
[8] Bard, P., et al., Frezenius Zeitschrift Analytische Chemie, Vol. 314, 1983, p. 25.
[9] Zeman, A. and Bartl, P., Frezenius Zeitschrift Analytische Chemie, Vol. 316, 1983, p. 43.
[10] Zeman, A., et al., Thermochimica Acta, Vol. 80, No. 1, 1984.
[11] Centers, P. W. and Smith, H. A., Journal of Synthetic Lubrication, Vol. 1, No. 3, 1984, p. 176.
[12] Coates, J. P., "Structural and Chemical Characterization of Neopentyl Polyol Esters by Infrared
Spectroscopy," ASLE Transactions, Vol. 9., No. 2, 1985, p. 185.
[13] Jones, W. R. Jr. and Morales, W., Lubrication Engineering, Vot. 41, No. 1, 1985, p. 22.
[14] Pachuta, D. G., et al., "Modern Methods of Turbine Fluid Analysis: Comparative Study of Several
Commercial MiI-L-23699Products," presented at the Aerospace Technology Conference, Society
of Automotive Engineers, Long Beach, CA, October 1985.
[15] Kauffman, R. E., et al., "Assessment of Remaining Lubricant Lifetime," November 1986, UDRI-
TR-86-14, AFWAL-TR-86-2024, Dayton Ohio Research Institute, Dayton, OH.
[16] Pachuta, D. G., et al., "Determination of Total Antioxidant Capacity in MiI-L-23699 Aviation
Turbine Oils by a Dynamic Differential Scanning Calorimetric Method," presented at the 26th
Eastern Analytical Symposium, New York City, NY, Paper No. 254, September 1987.
[17] Eisentraut, K. J., et al., Analytical Chemistry, Vol. 56, No. 9, 1984, p. 1087A.
[18] Stecki, J. S. and Kuhnell, B. T., Lubrication Engineering, 1985, Vol. 41, No. 8, p. 485.
[19] Rippen, M. E., et al., "Laboratory Spectrometer for Wear Analysis of Engine Lubricants," P &
W/ED FR-18951, AFWAL-TR-85-2101United Technologies Corp., Pratt & Whitney Engineering
Div., April 1986.
[20} Pachuta, D. G., et al., "Experiences with a Sequential ICPES System Applied to a Commercial
Flight Evaluation Study," presented at the Pratt & Whitney Spectroscopic Oil Analysis Conference,
West Palm Beach Gardens, FL, March 1987.
[21] Pragnell, J. W. A. and Von Tilberg, J. E., "Gas Turbine Oil Monitoring Programme," Paper No.
871014, Society of Automotive Engineers, Warrendate, PA, April 1987.
[22] Roberton, R. S., Lubrication Engineering, 1986, Vol. 42, No. 8, p. 466.
[23] Kight, R., "The History of NOAP in the Military," presented at the Pratt & Whitney Spectroscopic
Oil Analysis Conference, West Palm Beach Gardens, FL, March 1987.
[24] Suess, R. R., "Spectrometric Oil Analysis--A Current Overview," presented at the Pratt &
Whitney Spectroscopic Oil Analysis Conference, West Palm Beach Gardens, FL, March 1987.
[25] Humphrey, G. P., "The Development of Water Analysis as a NOAP Diagnostic Tool," presented
at the Pratt & Whitney Spectroscopic Oil Analysis Conference, West Palm Beach Gardens, FL,
March 1987.
Pontificia Universidad Catolica del Peru (Pontificia Universidad Catolica del Peru) pursuant to License Agreement. No further reproduct

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Copyright by ASTM Int'l (all rights reserved); Sat Sep 5 19:40:48 EDT 2015

Turbine Oil Monitoring

William C. Young and Reginald S. Roberton, editors

Turbine oil monitoring/William C. Young and Reginald S. Roberton,

Copyright 9 by AMERICAN SOCIETY FOR TESTING AND MATERIALS 1989

Peer Review Policy

Background and Development of ASTM D 4378: Practice for In-Service

A Turbine Lube Oil System Monitoring Program~D. BONETT 19

A Supplier's Approach to Turbine Oil Monitoring---G. R. TRABERTAND

The Reliable Control of Oil Quality in Japanese Turbine Units---

Monitoring Practices for Phosphate Ester Fluids for Turbine Lubrication

Experiences with an Analytical Monitoring Program Designed for

Background and Development of ASTM D

REFERENCE: Roberton, R. S., "Background and Development of ASTM D 4378: Practice

The involvement of A S T M in the preparation of an in-service monitoring practice for

Consultant, 497 Herrontown Road, Princeton, NJ 08540.

Purpose and Objectives

Turbine Oils--Their Nature and Composition

Study of Existing Practices

TABLE 1--Preliminary study of test methods in common use.

Test % of Users Using Test Comments

a Test Method for Neutralization Number by Color-Indicator Titration (D 974).

Format and Contents of Standard Practice

1. Type and design of system.

An equation for calculating turbine severity is included in an Appendix to the standard.

Quality Characteristics Which Must Be Retained In Service

Oxidation Stability Reserve

Freedom from Sludge

s Test Method for Oxidation Characteristics of Inhibited Mineral Oils (D 943).

Freedom from Abrasive Contaminants

Development of the Monitoring Program

1. The sampling and testing schedule.

Sampling and Testing Schedule

TABLE 2--Sampling and testing schedule--steam turbine oils.

Test First 12-Month Operation Normal Schedule

Viscosity 1 to 3 months 3 to 6 months

TABLE 3---Sarnpling and testing schedule--gas turbine oils.

Test First 6-Month Operation, h Normal Schedule, h

Viscosity 500 500

Logging and Interpretation of Test Data

~ ~, "8 1"o 1"2 14

Taking Necessary Action Steps

Other Areas of Significance

New Oil Handling

A Turbine Lube Oil System

KEY WORDS: turbines, monitoring programs, lube oil system

Basic Monitoring Program

TABLE 1--Original test program.

Typical Conditions and Corrective Action

TABLE 2--Current test program.

Test Method Limit

Viscosity ASTM D 445~ + / - 10%

FIG. 1--Viscosity trend. E

', 2 ,~ ,I- ,.~= 6 --r.. v= ~., ~':~', I I 12 ~,3.. i 4 1.5. ~,E 17 I ~.

TABLE 3---Acceptance test criteria.

TESTS PRIOR TO OFF LOADING

TABLE 4---Particle count specification.

Micron Size Range,

10-25 25-50 50-100 100-250 >250

Class 4 (new oil) 10 700 1510 225 21 0

A Supplier's Approach to Turbine

REFERENCE: Trabert, G. R. and Schreuders, G. J., "A Supplier's Approach to Turbine

The Parties Involved