Grease Making PDF
Grease Making PDF
R. S. BARNETT
Research and Technical Department, Texaco Inc., Beacon, N.Y., 12508 (U.S.A.)
(Received May 14, 1970)
SUMMARY
Recent lubricating grease research and technology in the U.S.A. has been a
wide-ranging endeavor with fundamental research investigations on theories of
structure (including complex soaps), permeability, electrical measurements, and
electron microscopy adding much to the knowledge of grease structure. NLGI
Fellowship studies have contributed significantly to this phase.
Outstanding advances have also been made in manufacture and processing,
giving greater efficiencies, shorter times of manufacturing and culminating in the
first truly continuous manufacturing process. Radioactive tracing of additive mixing
has been accomplished. Packaging has advanced with new materials, and new
ingredients for greases have become available. Inventory and quality control has
been marked by the use of computers.
Mechanical testing and evaluation has been a major effort in supplementing
simple non-bearing bench tests by providing laboratory rig tests using actual bearings
and gears. Many new designs of testing equipment have been developed, and studies
of the friction, wear and e.p. properties of lubricating greases, including ball joint
testing, have been extended.
Analysis and non-mechanical testing endeavors have included a critical look
at the significance of the bomb oxidation test, the development of an instrumental
method to measure color, and the use of infrared techniques for quantitative analysis
of lithium soap in lubricating grease.
Studies on flow and dispensing have been particularly active resulting in an
advanced understanding of grease flow, both theoretical and in practical applications.
In particular, apparent viscosity determinations have been correlated with flow in
pipes in a very useful way. A continuing development of centralized lubricating
systems has made for efficiency, economy and safety, and great expansions in bulk
handling have come about through better understanding of grease flow.
Formulation of lubricating greases has been marked by development of new
thickeners in addition to complex soaps, and in the expanded use of molybdenum
disulfide as a solid-film lubricating additive. The development and study of products
for extreme environments including aerospace applications has resulted in some
industrial spin-off. The new NLGI Reference Systems provide samples of the same
* Paper presented at the Institution of Mechanical Engineers Symposium on The Use of Grease
as an Engineering Component, London. Feb. I9--20th 1970. Published by permission of this
Institution.
Wear, 16 (1970)87-142
formulation and manufacture wllich can be used for research and evaluation l)!
laboratories with assurance of continuity, this being particularly valuable for co-
operative investigations by technical societies. Yew discoveries have been nlade wit11
old ingredients, such as the finding that l~igl~-soap-content greases givt> longer ball-
bearing lives. A special grease has been formulated for the food industry.
The application of lubricating greases and requirements for them have been
marked by the development of rustproof applications from the “inside-out” rather
than simply applying an asphaltic undercoating. The new cease-petroIatu]ll-t~ll~e
products applied mainly with airless sprays have given much better rust protection
for the life of the automotive vehicle than was obtained previously. Lubrication
intervals for automotive chassis greases have continued to increase, although certain
makes of cars have reverted to shorter periods and more grease fittings particularly
when conventional greases are used. There has been an intensive development of
aerospace applications with special greases such as the perfluorinated types coming
into the picture where hard vacuum, high temperatures, and other extreme condi-
tions must be resisted. However, it has been found that more conventional greases
may work surprisingly well, not only where sealed against vacuum, but in vacuum
environments. Improvements have been made in railroad lubrication particularly in
the understanding of the functioning of journal roller bearing greases and effect of
vibration on them, and the trend toward mild-e.p.-gear-oil traction-motor gear
lubricants which give better heat transfer, resist thickening, and afford improved
lubrication of gears.
The issuance of a revised NLG1 G~ossu~~) containing approximately IOOterms
now agreed upon in the lubricating grease industry should help the understanding of
these products by users and others. The hrLG1 Grade Classification has been made an
American Standard and is being considered for international standardization.
Production surveys made pe~odic~Iy by NLGI and recent nlark~tillg forecasts
have resulted in very helpful statistics and the recognition of trends. Considerable
thought has been given to better marketing techniques.
INTRODI2CTION
Historical
No review on U.S.A. articles on lubricating grease would be complete without
a mention of BONER’S comprehensive book1 published in 1954 which describes the
manufacture and application of lubricating greases to that time.
HOTTEN’S article2, an excellent, provocative critique written with keen
perception and wit, contains 339 literature references including patents and covers
the field to 1964. A companion article3 is that of BOLLO AND WOODS. This helpful
publication describes developments more recent than the BONER book, especially in
manufacturing and testing.
.%Clpe
The paper at hand summarizes U.S.A. lubricating grease literature as published
in the NLGP Spokesman and the two publications of ASLE** (Lubrication Elzg. and
* National Lubricating Grease Institute.
** American Society of Lubrication Engineers.
ASLE Tram.). It covers, primarily, the years 1963 to the present although a few
earlier papers have been included because of their outstanding nature. Some preprints
from the 1968 NLGI Meeting and the 1969 ASLE Meeting are included.
Theories of structure
Theories of grease structure have been marked by the varied NLGI Fellowship
studies, the studies of MARTINEK,KLASS AND HAINES~-6 on inorganic-thickened
greases, and also the application by BRIGHT798of electrical measurements to elucida-
tions of grease structure and apparent viscosity.
NLGI instituted, in 1951, their first Fellowship contract with the University
of Southern California. The awarding of Fellowships was temporarily suspended
following the grant which ended in 1968. ARMSTRONG~ and members of the NLGI
Fundamental Research Subcommittee have reviewed and appraised this activity
which has been aimed at a better understanding of the colloidal structure and funda-
mental properties of lubricating greases. Fifteen papers have been published in the
Spokesmalz in the years 1949-1969 as a result of these fellowships, including work
under the direction of M. J. AND R. D. VOLDof the University of Southern California,
EYRINGof the University of Utah, and SLAVERY of Northwestern University. These
investigations have contributed significantly to a better understanding of lubricating
greases.
The paper published concurrently with ARMSTRONG’S review was by MILES,
MILES, GABRYSHAND EYRING10 of the University of Utah on stress-relaxation and
recovery time for grease and polymer systems. Stress relaxation is the increase in flow
of the lubricating grease under stress attributed to the disentanglement of the
thickener fibers or particles. The tendency to return to the original state upon
cessation of shear is called recovery time, and is a measure of the thixotropic nature of
lubricating greases. This work has confirmed in some measure the Hahn, Ree and Ey-
ringtheoryforthisstressandtime-dependententanglement-disentanglementtransition.
The fellowship was returned to the University of California and the VOLDSin
1964 and they presented11 their ideas concerning research on grease structure which
would be pursued in the reinstituted fellowship. They described differential thermal
analyses on two samples of lithium soap greases of identical composition, one prepared
by quick cooling and one by slow cooling. The rapidly cooled sample when worked
gave a typical grease structure while the slow-cooled sample was a granular syneretic
dispersion of soap and oils. The quenched (quick-cooled) sample with good grease
texture showed less perfect crystals than the slow-cooled sample indicating that the
quenched sample may have a greater number of junction points between the soap
particles per unit volume, primarily between exposed carboxy metal groups, and this
may promote a favorable grease structure.
LANGMAN,VOLD AND VOLD~~studied the penetration of a lithium stearate-
cetane system with various fluids substituted by perfusion for the original cetane.
There was no correlation between penetration and viscosity of the interstitial liquid,
or any other simple physical property examined. LANGMANet al. tentatively proposed
that mechanical working, in general, results only in a deformation of the soap network
rather than in its rupture and reformation.
W&Z+‘,
I6 (1970) 87-142
VOLD, U~tr AND BILP reported, based on differential thermal analysis studies
and unworked penetrations, that the continuous structure in a lithium stearate
grease is necessarily formed from the undercooled waxy form in order to give a hard
grease relative to others of the same lithium stcarate content. This work confirmed
earlier work that a small but significant increase in penetration is obtained when the
surface is oil-wet as compared with penetrating a “dry” surface.
MARTIWEKet al.” developed an electrostatic repulsion theory to explain the
structural stability of inorganic-thickened greases. The theory that such structural
particles are held together by H-O-H bridges, as held by others, is rejected by
MARTINEKet al., their reasoning being that when such structures are ruptured, the
water molecules would redistribute themselves making it difficult to explain the
almost instantaneous reforming of structure upon the cessation of shear. MARTIiYEK
et al. believe that there is an electrostatic balance in non-organic-thickened greases.
When the particles move, repulsive forces build up inversely with the square of the
interparticle distance, following Coulomb’s Law. By their theory the yield value is
primarily the sum of the maximum repulsive forces between particles being moved.
Factors such as particle size, concentration, surface state and the electrical properties
of the dispersing medium enter into this. The decrease in apparent viscosity with
increasing shear is explained by particle momentum overcoming the repulsive forces
separating the particles. ~~aintenance of structure in the presence of syneresis is
explained as particles maintaining the framework at higher interparticle distances
even though capillary forces are decreased enough to permit “bleeding”. MARTINEK
et al. conclude that their theory is qualitative, and it is not possible to measure the
charges on individual particles. Electrical properties of such greases are considered in
Part II5 of this series of articles. The third article” is concerned with methods of test
and apparatus details.
BRIGHT'S first paper7 concerns the effect of shear on the dielectric constant
and dielectric loss, including design of a special cell to measure capacitance. A 14%
lithium-soap grease shows a higher dielectric constant than its base oil. The dielectric
constant of the grease drops off at higher frequencies, but the oil dielectric constant
does not. The dielectric loss goes up with frequency for the 6% lithium-soap grease,
but goes down for its base oil. For inorganic-thickened grease (modified clay) the
dielectric loss does not increase with the frequency, thus showing the difference in
dipolar characteristics between soaps and postulated spherical particles of inorganic
thickeners. The more random the structure, the higher the dielectric constant, as the
effect of shear is to orient the soap particles which perhaps reduces the capacity to
store electrostatic charges. One interesting point here was that a sudden cessation of
shear showed a rise in dielectric constant as the structure recovers from the orienta-
tion induced by the primary shear and reforms its disoriented and more random
structure, Continued constant shear produces a rise in dielectric constant (more
sharply for the inorganic-thickened grease) with time; here again indicating that
there is some shredding of the fiber in the case of the soap and breaking of agglomerates
or chains in inorganic-thickened grease, thus giving back the capacity to store electro-
static charges.
BRIGHTS continued the above work on four soap-thickened greases, inVeSti-
gating the effect of temperature changes on dielectric constant and also studying
points of inflection comparing dielectric constant-temperature data with apparent
viscosity-temperature data, the latter being measured with the Trident Probe
apparatusld. It was of interest here that both types of curves showed inflection points
or actual changes in direction at closely corresponding temperatures for a number of
products. The nature and magnitude of the changes occurring in the systems require
further work to interpret them and to determine the importance of such changes in
the use of greases as lubricants.
There has been much interest in the study of the permeability of lubricating
greases during the period covered by this paper, with ten publications appearing. The
pioneering work of SISKO AND BRUNSTRUM~~indicated that lubricating grease would
act as a permeable mass similar to the permeability found when water goes through
sand filters and oil through reservoir rocks. These flow processes having been found
to obey Darcy’s Law.
where B is the permeability of the porous media (cmz), U is the nominal velocity of
flow (cm/set), L is the depth of the porous bed (cm), q is the viscosity of the fluid
(poise) and P is the pressure drop across the bed (dyneslcm2). B is, of course, the
coefficient of permeability and is related to the free cross-sectional pore area of the
permeable material.
These studies relate to a fundamental property of lubricating greases, namely
leakage or oil bleeding; also permeability studies offer elucidation regarding the size
and shape of thickener particles. EWBANK, DYE, GARGARO, DOKE AND BEATTIE~~
made quantitative studies which bore out the earlier SISKO AND BRUNSTRUM ex-
ploratory work and confirmed that grease systems obey Darcy’s flow equation.
Strong interaction of van der Waals type forces between thickener particles and fluid
appear to change the structure and, coincidentally, the permeability, especially when
the greases were permeated with non-petroleum fluids, though not predicted by
Darcy’s law. Permeability is affected by type and amount of thickener, degree of
homogenization, mechanical working and type of fluid used. The relation between
bound and unbound oil in a lubricating grease is being studied.
BROWN AND EWBANK~~ studied the effect of non-soap (silica and coated
bentonite) thickener concentration and concluded that permeability represents the
area of the larger pores which serve as channels for essentially all of the flow. Perme-
ability is dependent on thickener concentration with good correlation obtained for a
two-coefficient equation of the form 3 = Ae-*C
ZAKIN AND Tuls studied permeability to help understand the rate of oil
separation from lithium-calcium greases and organo-clay greases made from naph-
thenic and paraffinic oils. Both types of greases had permeability coefficients in the
same range (about 3-IO.IO-I1 cm2) as for other greases. Both thickener types made
from naphthenic oil blends showed increases in permeability coefficients with increase
in viscosity indicating an increase in thickener particle size for these conditions; how-
ever, the paraffin&z oil greases showed much less variation with oil viscosity. ZAKIN
AND LIN’~ found that greases made from the same ten oils but thickened with two
types of silica differing in surface area, gave permeability coefficients varying from
12.6 ~1o-ll-24.0.1o-ll cm”. The two silicas gave about the same results, but their
paraffinic oil greases gave higher permeability values than those made with naph-
thenic oils of the same 77°F viscosity.
The importance of this work was recognized by NLGI, and a subcommittee on
pernleability was formed by the NLGI Technical Committee in 1961 with E~%QJK
as Chairman. This work was summarized by EWBANK in 196520 and it was concluded
that permeability is a basic measure of the leakage characteristics of the lubricating
grease itself, independent of the physical situation in which the grease is found, and
that permeability coefficients are affected by how thickener particles are joined to-
gether as well as by their size and number. The following findings give the consensus
of published work of members of this committee.
(I) Lubricating grease does obey the Darcy equation, with a permeability
coefficient which is independent of changes in fluid viscosity, thickness of grease cake
and pressure gradient, but which is materially affected by a change in the nature, size
or arrangement of the thickener fibers.
(2) The permeability coefficient of a lubricating grease is unaffected by
temperature, although the flow rate (and leakage) will increase with increasing
temperature due to the lower viscosity of the permeating fluid.
(3) Both soap- and non-soap-thickened greases exhibit permeability coeffi-
cients, thus indicating an over-all similarity in the nature of the thickener structure.
(4) In both types of lubricating greases, where manufacturing methods are
closely controlled, the permeability is inversely proportional to the wt. O, of the
thickener, the mathematical form of the relationship being logarithmic:
le-k f%?‘)1
Permeabilitv ti = A i
A and k are coefficients dependent on the nature of the thickener, and there is a
preliminary indication that k is a function of the shape of the thickener particle.
(5) Permeability coefficients have also been found to be dependent on the
type and viscosity of the lubricating fluid from which the grease is made, thus
indicating that there is sufficient inter-particle action between the fluid and the
solid to affect the manner in which the solid particles come together to form the
thickener matrix. This gives experimental verification to opinions long held by
greasemakers that certain types of grease would form properly only if a particular oil
was used as the vehicle. The effect has been shown to occur both in soap-thickened
and in inorganic gelled greases.
(Reviewers note: While repeatable results have been obtained by committee
members in their own laboratories, interlaboratory reproducibility has been unsatis-
factory, and so the above work has been suspended by NLGI with the understanding
that the technique is a useful tool for studying leakage and structural differences
within one laboratory. A summary report on the NLGI work will be published in the
Spokesman.)
WEBSTER AND EWBANK~~ have confirmed the EWBANK AND BROWN relation-
ship that there is a non-linear function between thickener concentration and perme-
ability which has a different value for non-soap thickeners as compared to soap
thickeners.
MCATEE AND CHEN~~ studied the effect of thickener concentration, organic
dispersant concentration, aging and temperature on the permeability and penetration
of an org~o-montmo~~onite-thickened grease. It was found that pe~eab~lity
varied with thickener content indicating different structures for the higher amounts
of thickeners. A possible explanation was that the number and degree of particle-
particle bonds increases to a maximum at about 7% thickener. Above this there
continues to be a great deal of particle interaction, but micropores or channels
develop which lead to the increased permeability. This may be due to less-than-the-
optimum amount of dispersant at the higher thickener concentrations. The effect of
temperature may be to break up aggregates allowing more structure to be built, but
increased thermal energy allows the individual interactions to be weaker which is
shown as a general decrease in both permeability and gel strength.
MCATEE AND FREEMAN~~ studied greases thickened with organo-mont-
morillonite, organo-hectorite, asbestos, asbestos-organo-montmorillonite and silica.
It was indicated that asbestos gave the most open structure with respect to the flow
of fluids through the network, while the organo-montmorillonite results in the least
porosity. Correlating this with structure, asbestos with the smallest surface gives the
largest permeability, whereas the plate-like particles of the organo-montmorillonite
give the least permeability. The lath-shaped organo-hectorite was intermediate in
permeability. MCATEE~~also showed that permeability measurements are valuable
in studying the addition of dispersants and the important structural effects of small
amount of water on organeclay-thickened greases; also, permeability measurements
give information on how dispersants affect the worked stability of greases.
Complex thickeners
The NLGI Glossary (3rd edn., May, 1968) defines complex soap as “a soap
wherein the soap crystal or fiber is formed by co-crystallization of two or more com-
pounds :
(I) the normal soap (such as metallic stearate or oleate),
(2) the complexing agent. (Examples of complexing agents are the metallic
salts of short chain organic acids such as acetic or lactic, or the inorganic salts such as
the carbonate or chlorides. The complexing agent brings about a change in grease
characteristics usually recognized by an increase in dropping point.)
HOTTEN’Sexcellent review2 summarizes the situation well, including his com-
ments on POLISHUK’Scomprehensive paper25 on calcium, barium, and aluminum com-
plex soaps. HOTTENpoints out that a I : I acetate-stearate molecular ratio in calcium
complex greases seems to maximize some properties, such as raising the dropping
point to above 500°F. However, with “super complexes” of higher ratios of acetate,
it is not clear that these are definite chemical compounds as brought out by the earlier
work of PANZER~~.Electron microscopy showed distinctive crystals for the calcium
acetate-stearate complex as compared to different shapes for calcium acetate and
calcium stearate alone. POLISHUK~~thinks that complex soaps are definite chemical
compounds which can only be formed by polyvalent metals. The picture needs further
research to clarify the exact or inexact nature of these complexes. High-melting
complex aluminum soaps as grease thickeners are said to overcome the poor dispensing
properties of calcium complex greases, and the aluminum complex greases show good
mechanical and thermal stability and are reversible. Barium complex greases need
about 30-45% soap, calcium complex greases require 15-250/~ soap while aluminum
complex greases need only about 3-8% soap owing to the very small fiber size of the
Al complex soaps.
W&Z+‘,
I6 (1970) 87-142
BARRETTE ASI) G~K~AI,E~~~ studied characteristics of lubricating greases
from calcium salt-and-soap complexes synthesized in different reaction media, thcsc
ranging from low-boiling alcohols to highboiling aromatic hydrocarbons such as
xylene. The nature of complexes are not given as they were formed from unspecified
ratios of long-chain fatty acids, short-chain fatty acids and acetic acid neutralized
with unspecified amounts of calcium hydroxide and caustic soda. No analyses of the
thickeners are given. Electron micrographs showed different sizes and shapes for the
thickeners synthesized in various reaction media. However, infrared spectra indicate
no chemical differences occur by making the thickeners in different reaction media,
indicating differences in grease properties found were due to variations in physical
size and/or shape.
Miscellaneous
P,ZKZER”~ has modified and combined theoretical equations from the literature
for nucleation and growth rate of crystals to obtain the effects of certain reaction
variables on the rate of particle size change. Under grease-making conditions, the
equations show that the average grease-thickener particle size is reduced as the
following are decreased: reaction temperature, thickener concentration and oil
viscosity. The predicted results correlate with numerous experimental results reported
in the literature, therefore the equations can be used to guide grease manufacture to
achieve a particular size distribution or shape. Factors affecting free energy, such as
oil composition and surfactants, are qualitatively indicated to be more important than
variations in temperature or supersaturation.
The chemistry of aryl-substituted urea (_4SU) thickeners has been extended
by TRAISE~” whose work indicates that a linear polyurea is the actual thickener in
ASU greases which results in improved grease properties. Both aliphatic and aro-
matic polyureas were studied as thickeners, as well as aliphatic-aromatic mixed
types.
CALHOUN30has studied grease bleeding in some depth, showing that high oil
bleeding correlates with high permeability coefficients for the same greases. This
confirms earlier thinking that the oil component of a grease is held by (I) molecular
attraction of the thickener and polar oil components, (2) capillarity and (3) possible
mechanical entrapment in some greases. Molecular attraction is postulated to hold
some 20-25 y& of the oil in a grease, which can be removed only by solvents. Capillary
forces may hold some 751;) of the oil, of which about 113can be extracted by gravity.
The remainder can be forced out by externally applied forces of sufficient magnitude.
ZAKIN, LIN AND Tc31 used a permeability cell to explore sorption and extrac-
tion of an additive (0.5-3.07;) in lubricating greases. It was found both for lithium
and modified-clay greases that the additive (phenyl-ol-naphthylamine) was partly
associated with the thickeners and partly dispersed in the oil phase of the grease, with
considerably more additive associated with the modified-clay surface than for the
lithium hydroxystearate soap. Extraction with additive-free oil removed the additive
from the thickeners almost completely from the lithium greases, but left a small
amount (about 0.2Yb) in the modified-clay greases. Constants for exponential equa-
tions describing the initial rates of sorption and extraction were evaluated. For each
type of grease, the average values of these constants were about equal.
HOROWITZ END sTEIDLER3" made a digital computer analysis of the effects of
MANUFACTURING,PROCESSINGAND PACKAGING
Packaging
LANGNER@ described changes or modifications in frequently used grease
packages in a well-illustrated article ; semi-bulk packaging and bulk grease handling
equipment were also described.
The Fair Packaging and Labelling Act is discussed by SCHNEIDERHAN~~ which
requires that consumer commodities be clearly labelled as to quantity of contents,
nature of ingredients, etc. Such products as antifreeze, automotive chemical products,
LPG, home lubricants, motor oil, solvents and cleaning fluids were ruled to fall
within the consumer commodity classification when this paper was presented in
September 1968 ; appeals are pending on rulings.
wATTS4s tells of the anti-corrosion and dent-resistant properties and leakage
resistance of rigid polyethylene containers.
GILBERT AND CATANZARO~~discussed materials, manufacturing and quality
control of grease cartridges and their filling and distribution for various markets.
NIDF,S~~ discusses the capabilities of the steel container industry and the work
of the Steel Shipping Container Institute. Eighteen million pails and 8.5 million steel
drums, are produced every year for the petroleum industry.
Miscellaneous
Private carriage is attractive to industries, particularly where back-haul can be
employed according to ALEKSA~~.
FRIEDE AND SANGSTER~~have compared six oil bleeding tests run on 17 greases
with varying soap base, soap content, oil viscosity and texture. ASTM D 1742 and a
centrifugal test were found to give the best correlation of static oil separation under
field conditions. The centrifugal test is well-adapted for routine quality control, being
rapid, reasonably sensitive and simple. CROFTER, Chairman of I.P.Panel St-D-r
Wear, 16 (1970)87-142
RECENTUSA PUBLICATIONSON LUBRICATINGGREASE 97
General Tests (Greases), has commented on this paper and pointed out that I.P. 121,
which is one of the six tests considered, has been used to set a 2% maximum for
bleeding of those greases which would generally be satisfactory in storage. The 17
greases examined by FRIEDE AND SANGSTERwere satisfactory regarding separation in
storage. The I.P. method is a screening test only, to show that badly made greases
would give excessive oil separation in storage. The author’s response acknowledged
the clarification given by CROFT, but stated that tests requiring less than the 7 days
required for 1-P. 121 are helpful at times.
CAWLEY~~discussed lubricants plant scheduling and inventory control etc. by
computer; benefits of these programs are discussed.
Quality control in compounding and blending lubricating oils and greases has
been reported by GEBHART~~.Quality control starts with development of a new
product and continues through manufacture and confirmation of the finished product.
Also, quality must be protected in storage, shipping, and in application to realize the
full benefits obtained. Specifications of raw materials are also important. The func-
tions of the quality control laboratory in a large plant are described.
GRAHA~M~~ reported on efficiencies and costs in US grease manufacture in a
paper presented in 1965. Actual manufacturing was observed in the grease plants of
five different companies; a total direct cost summary (Table VI of the paper) is
given. The manufacturing costs developed by GRAHAMaccount for only 3-g% of the
total direct cost figures.
CORSICAreported on the general properties of commercial fatty acids, giving
physical and chemical characteristics. A sequence of description of raw materials,
conversion of fatty acids and separation of fatty acids were outlined. Specifications
are defined and routine analysis and composition of commercial stearic and oleic
acids are described. In 1960, 23.4 million pounds of fatty-acid soap were used in
lubricating greases.
COENENANDGORDON59describe the radiotracer mixing of additives in grease.
This interesting study determined variations in additive concentration made in in-
line blending facilities, and also additives blended with kettle-mixing facilities in
which hydrocarbon-soluble and hydrocarbon-insoluble additives were blended. A
radiotracer technique using radioiodine was used.
SINGH@Jreported in 1965 on the manufacture of lubricating grease in India
and aspects of applications. This survey-type article presents an interesting historical
section of the progress in India from the settlement of Aryans about 5000 B.C. to the
present, including the continuing lubrication with ripe bananas of some IO million
bullock carts in use today, in areas which grow this fruit. Bananas also were used for
the launching of ships as recently as 1955. Concurrent with the indust~alization of
India, the use of modern lubricating greases has grown ; however, animal fats are
unacceptable because of religious beliefs. Native lubricating grease production uses
fatty materials of vegetable origin. The local manufacture of grease started over a
decade ago with production of calcium-soap cup greases using Mowrah fatty oil and
imported lubricating oil stocks. It is hoped in the next decade to satisfy India’s grease
requirements from almost 100% mdigenous
’ components. Modern grease plant facilities
have been developed within the last decade.
Ttre testing of lubricating greases on bearings and gears in laboratory rigs can
be thought of as a trial marriage in which new grease compositions meet the hard facts
of life for the first time in the type of mechanism with which they will ha.ve to live.
Analogous are such factors as compatibility, the overcoming of friction and noise,
and the ability to perform smoothly so that fretting and attrition are held within
bounds. Once these things are established, it is time for the continuation of this trial
into the field where even more stresses and strains and environmental difficulties are
imposed. Finally, the successful candidate is ready for its destiny of marriage with
components in full-scale service.
A comprehensive publication is that of SCHILLING~~I~"reprinted from the
Revue de L’lmtitzlt Fraracais du P&role, which examines a large number of test rigs
developed in Europe and in the USA. These are mostly ball- and roller-bearing rigs,
though a gear wear test is mentioned and also the four-ball, ring-and-block and pin-
and-bushing types of e.p. tests. These articles are particularly valuable for their
concise descriptions of each rig together with a schematic drawing illustrating the
basic design in each case. Problems raised by mechanical tests, and the properties of
greases and their components important in the lubrication of rolling bearings are
discussed. A sumn~ary of grease specifications {mostly military) as of 1963 is given. A
summary of the principles and potentials of some mechanical tests and trends in
grease lubrication are also discussed. SCNILLING concludes that the tests outlined are
very complex but necessary because of the shortcomings of simpler classical tests. The
importance of international studies is mentioned and the need to conduct research on
the fundamental properties of grease structure, flow, etc. is mentioned.
Wea?‘.16 (1970)87-142
The demands of the military for the lubrication of advanced aircraft and spare
vehicle components has stimulated research and evaluation of lubricating greases
extensively in recent years. MCCARTHY Go describes a high speed-high temperature test
rig for grease-lubricated ball bearings giving detail, design features, instrumentation
requirements and operational characteristics of a rig developed under an Air Force
contract to test greases under the following conditions: size 204 ball bearings, speed
up to 45,000 rev./min (maximum of 900,000 DN Value), and with operating tempera-
tures from ambient to Ooo"I;, and under radial and/or axial loads up to rjo lb.
Continuing the studies of greases for aerospace, SLINEV ASD JOHNSON?O
present preliminary evaluation of greases to boooF and solid lubricants to 15oo*F in
ball bearings. Perfluorinated alkyl ether greases with telomer or organic dye thickeners
were satisfactory lubricants up to 500°F for the 440-C tool steel slave bearings used
in this special test rig. These were size 204 bearings run at speeds of 2,000 and 5,000
rev./min (see section on aerospace lubricants, pp. I 23-128).
HOWELL described initial experiments with a ball bearing simulator (BBS),
basically a three-ball thrust bearing with flat disc races. One race is motor driven
and the other is restrained from turning by a torque-indicting system. The balls are
constrained by a cage arrangement supported in miniature bearings. A lithium soap-
mineral oil grease and a lithium soap-synthetic oil product were screened on the BBS
for comparison with gyro life and with memory-drum life with qualitative correlation
obtained indicating the mineral oil grease best. Furey questioned the details of deter-
mining electrical resistance between the moving surfaces (used to give an indication
of film thickness on the raceways), and this was commented on by the author.
The flow of grease in prepacked rolling bearings, has been studied by
LANGSTRBIC by means of a removable section of the outer ring. The rollers and cage
appear to act as pump elements which circulate adjacent grease through the bearing
where it softens, lubricates and removes wear particles from initial running-in. Shear-
stable lithium greases may allow almost full packing of the bearing without shear
breakdown of the bulk grease. This promotes longer life without relubrication.
Wenr, r6 (1970)87-142
RECENTUSAPUBLICATIONS ON LUBRICATINGGREASE 101
damping characteristics of the bearing are influenced by the lubricant used and
lubricants behave differently in this respect. Various vibration tests with a number of
greases are described and data indicate a substantial effect on the bearing vibration
level in the frequency range between 300 and 10,000 Hz. Grease effects are more
pronounced for smaller than for larger bearings. Higher penetration (softer grease)
correlates significantly with a decrease in vibration level. Preworking greases in a
3-ball grease worker may either raise or lower the vibration level.
BERUSCH AND KINGLY reported on the Naval Ship Engineering Service
Program for improved quiet-bearing lubrication. This work was considered necessary
because of noise problems in auxiliary machinery of submarines. Using both vertical
and horizontal rigs at two laboratories indicates a lubricating grease-ball bearing
interaction which can result in high vibration levels. The hotter running the grease,
the greater the tendency toward high vibration levels. The type of loading, load
amount and temperature levels affect grease-bearing vibration life. An objectionable
increase in vibration in horizontal rigs accompanies an increase in temperature of
some 18°F and this marked also the lubrication life as determined by a complete lack
of grease in the frictional zones. The vibration life of a grease-bearing combination is
equal to total performance (lubrication life) in the horizontal test rigs, whereas
vibration life was equivalent to 5o-qo’$ of the total performance life in vertical test
rigs depending on the grease used. Specification MIL-G-24139, quiet-running grease,
is an outgrowth of this work.
The article by LIESER AND WESTON, previously discussed, bears on the effect of
externally imposed vibration on grease structure and consistency.
Miscellaneous
CHASE, SANDMANN AND SAVIDGE~~ studied evaluation of lubricants and coatings
for the prevention of thread galling and seizing on
17 lubricants and 7 bolt/material
combinations. Stress corrosion effects of lubricants on bolt materials for use at 4oo”-
550°F external applications were studied. The lubricants, covering a wide range of
solid-film lubricants dispersed in various carriers, did not cause stress corrosion
cracking: however, pitting was noted on certain alloy specimens. Grease-type lubri-
P~~s~~a~ testifzg
This category is rather limited as compared to the extensive work on mechani-
caltesting, but analytical efforts were marked by an infrared quantitative analysis
method and also a development of a leakage test using principles of permeability.
BIJTTLAR AND CAxTLEk-$1 developed a quantitative infrared method for
lithiu~l-soap lubricating greases, specifically lithium Iz-hydroxystearate greases.
Past infrared studies have been mostly qualitative on components. Physical charac-
teristics and homogeneity of the soap fiber system, and therefore crystallization
techniques, affect the absorption of infrared radiation. This method uses a controlled
recrystallization technique.
Chemical tests
DREHER, CRIDDLE AND KOUNDAKJIANQ~ questioned the significance of the
ASTM oxidation stability test for lubricating greases. Method D 942 stems from work
in 19x6 by Wright and Mills. It has been standardized for 15 years and in use over
20 years. DREHER et al. contend that its significance remains to be established. Data
show that pressure drop is not a direct measure of oxygen absorption in that greases
produce gases as oxidation proceeds. Therefore, more oxygen can be absorbed than is
shown by the pressure drop in some cases. Additives may lower bomb oxidation
ratings. Dynamic bearing tests in oxidizing environment are considered much more
indicative of performance of greases. Discussions by BOOSER ANDGROSSETT~~con-
tradict DREHER et al. in some degree. Correlation with ball bearing grease life is shown
by BOOSER for a number of greases, and the use of D 942 in specifications for assuring
good storage life is upheld by GROSSETT where similar grease types are compared to
estimate either static performance or shelf life.
MCKIBBEN ANDFORINASH~OO have related humidity-cabinet life of lubricants
to their service life. A method expressed mathematically as a function of temperature,
* Now Division.
Miscellaneous
CARTER AND BALJMANN~~~have reported on the gas chromatography of fatty
acids applied to grease formulation. The composition of such acids used in preparation
of thickener soaps importantly affects the grease properties, and examples are given.
New analytical techniques such as gas chromatography permit close control of fatty
acid compositions, and therefore insure uniformity of quality.
CRIDDLE~~~ discussed the use of an electronic counter to study the size of
distribution of dispersed grease thickener particles. Electron-microscope (e.m.) photo-
graphs of thickener particles may not be representative of the particle size and shape
distribution and conclusions are based on observations of less than o.o10/ of the total
solids of the sample. This causes doubts concerning the typical nature of e.m. photos.
Electronic counting emphasizes the larger particles and detects about I-85% of the
total solids; however, size distributions depend on concentration, age of the disper-
sion, and the shearing process. Particles counted were larger than 2 rums. The method
supplements electron microscopy.
JACKSON~~* developed techniques for handling greases and other semi-solid
substances. For greases, a suitably sized sheet of polyethylene is taken and the re-
quired weight of grease molded into a roughly cylindrical shape near one of the longer
sides of the sheet, which is then rolled into a tube, tapered if necessary, and fitted
into the neck of the flask. The grease is extruded by squeezing downwards from the
other end. The amount of sample taken is determined by weighing the flask or tube
before and after the introduction of the sample. A water determination (Karl Fischer
method) can be run using this technique on a IO g sample with less than 0.2 mg water
being introduced during the time the titration vessel is open to the air.
The years covered by this review have been fruitful both in understanding
lub~cating grease flow and in applying this knowledge to such practical fields as flow
in pipes, centralized lubrication systems, bulk dispensing and in the measurement of
apparent viscosity at elevated temperatures.
where pg is the grease viscosity, s is the shear rate and ,um,b and m are constants for
any grease and temperature. This equation makes for easy comparison of the curve
of log viscosity vs. log shear rate obtained from ASTM Method D 1092 for apparent
viscosity. BRWSTRUM’S nomograph, given in the article, supplies the calculation of
pp from the constants, or the constants from the curve. It is also possible to calculate
the flow constants from the point data by using a modified approach to the nomo-
graph.
FARRIS AND SLATTERY~OSconsidered flow in an infinite journal bearing, this
being the first report on the NLGI-sponsored study of the movement of non-Newton-
ian materials in an infinite journal bearing. The work reported herewith concerns a
reanalysis of the coaxial coordinate model set up in terms of a Newtonian fluid. The
results are in agreement with a previous solution based upon a different approach in
rectangular Cartesian coordinates. The next phase will be a study of a variational
solution for a simple non-Newtonian fluid.
MORRISON~~~has reported on the relationships between the composition and
rheological properties of a series of lithium hydroxystearate greases made under
identical processing conditions but using different oils. Earlier work by Ellis had
shown that for a given method of preparation, the relationship between the worked
penetration at 77°F and the soap content of a grease is log penetration= A-B
temperature used in running the test. Correlation of Ventmeter readings has been
obtained with pipe supply line size and length. Possibilities for extending the appli-
cability of the Ventmeter are discussed.
Celztralized systems
There has been a great development of centralized systems for dispensing grease
in the last few years, representing a major advance in grease technology. Such systems
assure delivery of a positive amount of lubricant at the right time and in the correct
amount and also assure that every bearing is lubricated and that minimal contami-
nation will exist.
BERG, HORTH, NIXON, PANZERAND PLUMSTEAD~~~ have studied plugging in
centralized grease lubrication systems. A field survey indicated that a laboratory
screening test could be built that would predict relative performance in a variety of
field installations and also this could be accelerated to obtain useful results in a
reasonable time. It was found that design of metering devices, operating conditions
and grease characteristics all contribute to plugging; with the major grease factors
being consistency, oil separation (if this changes consistency to a large extent), and
the effect of additives. CALLAHANAND McDoLE~~~ comment on this paper to the
effect that straight lithium greases and calcium-complex greases are difficult to
handle in central systems because of separation; however, e.p. additives correct the
Dispensing of grease in bulk has grown tremendously in the last six years.
SPARKS AND TOVEY~~~ have discussed “Bulk Grease-rg62”, in a well-illustrated
article, pointing out that bulk grease handling at that time was nearly four years old.
Follow-up plates or mechanical agitation devices have not always proved necessary.
The author gives the following list of main points for a bulk-grease system :
(I) Keep fill and header lines as short as possible.
(2) Fill and header lines should be heat-traced, preferably with electricity or
low-pressure steam, and insulated if exposed to low ambient temperatures.
(3) Storage tanks should be in a heated area or insulated for better grease
slumpability.
Weav, 16 (1970)87--142
RECENT USA PUBLICATIONSON LUBRICATINGGREASE III
FORMULATION
ANDADDITIVES
IP, and NLGI, have been subject to a recurring objectionable happening, This stems
from obtaining round-robin samples from commercial production submitted 1,~.
volunteering members of the cooperating group. Therefore, when it came time to
repeat or run further round-robins, it sometimes happened that greases had changed
irom the time they were first offered, or were no longer available. This is understand-
able when commercial products are considered.
The need for a standardized set of samples or reference systems was discussed
at NLGI for some years and finally culminated in the formation of an ad lzoc Commit-
tee on Reference Systems in 1966, with the first batches of the Systems being made in
October 1966. The ad hoc group has now become the subcommittee on Reference
Systems of the NLGI Technical Committee and two products of 300-310
worked penetration have been made available to groups who wish to purchase
them. These, both made from the same mineral oil of about 300 SCS/roo"F, are
Reference System A, made with 4.7 (;!hlithium hvdroxystearate soap, and Reference
System B made from 6”; organic-coated-bentonite thickener. The only additive is
0.510 antioxidant concentrate*. EWBAKK, Chairman of this subcommittee, reported129
in 1967 on the development, details of formulation, and status of the systems.
Samples have been distributed widely, both nationally and abroad. Over one-half
the papers at the 1965 NLGI meeting gave data on the reference systems. Therefore,
this achievement is certainly filling a need. A second objective is to follow the storage
of the systems and to determine the degree of reproducibility of successive batches
made from the same ingredients. So far, no significant changes have been found.
Greases ~~?~~a~~~~~~
~~ly~de~u~ disufi‘hle
DEVINE, LAMSON AND STALLING 137 have reported on diester lubricating
weear,X6 (1970)87-142
greases containing Alo&. Their study indicates that MoSa increases lo:~d-carryir~g
capacity and reduces wear under heavy loads. No adverse effects on storage stability,
oil separation and antirust properties are given by the MoS2, whicll is confirmed b?;
good field performance, storage stability and corrosion protection. pl;o advantages arc’
given by smaller-particle-size RIoSz (0.3~0.7 ,um) over the lubricating grade &I(&
(6-7 pm) ; in fact, lower oxidation resistance was obtained using the former. (ireases
containing %Io!% and other sulfur compounds regenerate a lubricating film when
tested on a bearing assembly having a molybdenum metal component contrasted to
results in steel-steel bearing combinations.
BARRY AXL) BINKELXW~~X evaluated the effect of MoSa in a multi-purpose
lithium grease, this study being in three parts: load-carrying capacity, antirust
protection and oxidation-bomb stability. Increases in load-carrying capacity and
film endurance were found. Some effect of particle size is shown, with slow-sliding-
speed oscillation tests giving best results with larger particle size, (7 pm), whereas the
higher-speed constant-rotation conditions of the Timken machine reflect better
performance from the finer particle size (o.7 pm). It is indicated that MO& addition
decreased the oxidation rate of uninhibited soap and modified-clay-thickened greases.
Inhibited greases containing MOSS generally pass the ASTM D 1743 corrosion test,
with I”~ of an amine alkyl phosphate being effective in IO out of 12 greases tested.
RIWON AXI) BI~IEIJI,L~ r139 have studied the oxidation stability of un-
inhibited lithium-soap greases with and without MO& in the laboratory, and also
ball-bearing functional-life tests of various greases and pastes containing MoSZ.
Addition of IO’?; MO& particularly reduced the oxidation rates of lithium greases
made from paraffinic base oils, whereas varying the soap content from 8 to 12’j;, for
such greases had very little effect on the oxidation stability. An amine antioxidant
markedly reduced the oxidation of the naphthenic oil-&loSz grease bringing it up to
the level of the paraffinic oil MO& grease without antioxidant. ASTM D 1741 func-
tional life tests are lengthened by the addition of 10”; MO& to lithium, sodium,
calcium-complex, barium and modified-clay-thickened greases, but not for a calcium-
soap grease where poorer life obtained. In the ASTM D 1741 test at 25o”l;, pastes
made with MO& and mineral oil outperformed pastes made with MoS, and synthetic
oils; no jamming of the ball bearings was found in these tests.
RISUIJN ANI) SAI~C;EW~“” have published Part I of a comparison of commercially
available greases with and without )loS L, using Timken, I’alex, four-ball e.p. and
four-ball wear methods. Fifty-eight greases were submitted by 1 j manufacturers, of
lithium, lithium ra-hydroxystearate, calcium-complex, barium, and aluminum-com-
plex soaps and clay types, mostly NIX;1 No. 2 grade. One group contained e.p.
additives initially. In the Timken test method, no continuous-grease-feed apparatus
was employed and the level of Timken OK loads obtained was considerably lower
than that found by using ASTM D 2509 which specifies continuous feed. The overall
results basis Part I, on greases with and without MOST, indicate that calcium-complex
greases provide the best perfortnance in these bench-scale tests, with the remaining
greases performing moderately well. Ry these tests, performance of MO% greases
supplied by- the manufacturer was better than for the same base greases without
Moss, and uniformity of performance was better for the commercial MO% greases than
for the commercial base greases to which MO& was added. Laboratory blends of
commercial greases with I, 3, and IO:,; of MOST added, in general gave higher film
strength as reflected by Falex, load wear index, four-ball weld load, and four-ball
wear scar data. The load wear index (formerly mean Hertz load) was the most con-
sistent indicator of improved performance. Timken results were rather inconsistent
and insensitive to MO& addition. In general, benefits obtained by adding 0.7~,um
MoSz were greater than those obtained from 7-,um MO!&. Phase II of this work will
cover evaluation of the greases in the GMR laboratory ball joint test apparatus for
brine sensitivity and torque stability; as well as for fretting corrosion, corrosion, in
IOO~; humidity, and oxidation stability.
JOHNSON~~~ has reviewed the earlv use of molybdenum disulfide as a lubricant.
The first documentation of the probable*use of molybdenite as a lubricant goes back
to the early 16300's.The good surface adherence of MO& is attributed to strongmetal-
sulfur bonds ; the compound shears easily to give low friction because of the weakness
of the sulfur-to-sulfur bond. MO& performs best in the absence of contaminating
materials while graphite requires adsorbates such as moisture or oxides for its best
functioning as a lubricant. MO& is brought into intimate contact with the base
materials during the rubbing action of loaded mating surfaces. The largest volume use
of MO& is in greases. Small amounts of MoSa (less than 59&) in oils give very limited
improvement in reducing friction wear, probably due to preferential wetting of the
surfaces by the bulk liquid. In the last 25 years, several thousand world-wide technical
papers have been published on the use of MO& as a lubricant. The use of MO& in
bonded solid films, in-situ-formed films, pastes, and solid composites is also discussed.
KITCHEX'@ has reported on the use of molybdenum disulfide in the communi-
cations industry. A number of applications where MoSz has shown to be advantageous
are given for manufacturing and product experience, materials of construction,
service and maintenance and in new-lubricant formulations where conventional
lubricants are unsuitable. These range from the use of MoS&richloroethylene slurry
on rusty chain-sprocket arrangements in a vapor degreaser (where the rust particles
seem to bind the MO&) to use as a wear-in lubricant for large gears of the Telstar
antenna where the gear roughness was reduced from 300 to 145 pin. after two years
of service, using 5-7 pm (200-280 ,uin.) MO& in a heavy oil-soap mixture. Use of
MoSz paste in “flea-power” motors promoted long life and protected against corrosion
in tests under nearly IOO~~ relative humidity at 100-~40~F ambient. Cautions are
that solid MO& must have adequate clearance between rubbing surfaces, and that
uncompounded MO& should not be used under high humidity or highly corrosive
environments because of its absorptive characteristics; MoS2 is not a “cure all”.
Misceltalzeaus
SCHWARTZ~~Q reported in xg6z on the effect of penetration and thickener con-
tent on ball-bearing-grease performance, with very interesting findings. Considering
pairs of greases, similar in type and approximately identical in penetration, but
differing in thickener content, the non-milled grease with higher soap content gave
si~ificantly better performance in life tests than did its milled counterpart. In con-
trast, specification tests failed to show any significant differences between any milled
grease and its non-milled counterpart. Bearing temperatures were from 100°C to
175X, and speeds ranged from 3600 to 7000 rev./min in both open and enclosed
bearings.
DREHER, SMITHSON AND CARTER~~~reported on a special grease for the food
industry. The product is thickened with alu~num-complex soap and made from
USP white oil plus specific oxidation and rust inhibitors allowed by the Food and
Drug Administration. Details of the isolated equipment use in manufacturing grease
is given: extensive field tests were carried out successfully in can-making and canning
0.19 for all greases tested. A 60 ,uin. finished journal, when lubricated with a grease
of high viscosity base oil, runs at a lower torque than a IO pin. finished journal.
MITCHELL AND SnoRTRNi57 gave an interesting detailed account of the
development of a multi-purpose lubricating grease. Descriptions are given of the
various physical, chemical, and mechanical rig tests used in the United Kingdom to
develop greases, particularly for lithium-soap products, and some of the difficulties
which came up in trying to meet bearing manufacturers’ requirements with a single
product. The authors estimate that it took seven years and 40,000 research man-hours
and IOO,OOOh of mechanical rig testing plus field testing to arrive at their objective.
Details are given on European test rigs such as the SKF RzF tests and the Emcor
corrosion rig, the Ransome and Marles horizontal rig, in addition to the usual ASTM
tests. The reasons for finally ending up with a lithium-soap grease rather than other
thickeners are presented.
Automotive vehacles
For a number of years ELDRIDGE 158-163 has covered the lubrication require-
ments of automobiles at successive NLGI meetings. These have been very useful and
up-to-date articles on new engines, chassis lubricants and relubrication intervals, rear
axle lubricants, automatic transmission fluids, crankcase drain intervals and other
features such as exhaust-emission-control devices in 1969. These articles are well
illustrated with pictures and diagrams, and illustrate trends in lubrication from year
to year.
LANE AND FOELL~~~ considered the matter of extended car service in a 1963
paper, discussing extended lubrication intervals (ELI) which started in the USA
with 1961 automobile models. The pros and cons were discussed. In this connection
ELDRIDGE’S review for 1969 cars 163 shows relubrication periods ranging from 2,000
miles for Buick, if a regular chassis lubricant is used, to 36,000 miles for Chrysler and
Ford.
SAE* Information Report J3roa Automotive Lubricating Greases165 was re-
printed in the NLGI Spokesman in 1968 with the permission of SAE because of its
great pertinence to NLGI. Subcommittee 4, Lubricating Greases, of SAE, with LANE
as Chairman, prepared the report with the help of Subcommittee 4 and the Chairman
of the NLGI Technical Committee. This document, therefore, combines the agreed-
upon thinking of the automotive and petroleum industry members concerned with
lubricating grease. It is a concise primer of lubricating grease characteristics, perfor-
mance requirements and properties; and defines a number of terms and lists pertinent
grease tests which are mostly ASTM methods. Greases are designated by fields of use
in automobiles including wheel bearings, universal joints, chassis (both periodic and
extended-lubrication-interval types) and multipurpose greases. Grease application is
discussed and the relative importance of lubricating grease properties for automotive
uses shown.
MILLER~~~ reports on the “Chrysler Viewpoint-Lubrication 1963” pointing
out that extended lubrication intervals do not end the need for services of the grease
producers by the automotive industry and such cooperation may be increasing be-
--~
* Society of Automotive Engineers
w&W’, I6 {?g70)87-142
RECENT USA PUBLICATIONS ON LUBRICATINGGREASE 123
ture, better heat transfer from the gears to the gear case giving cooler operation of
the gears, more accurate measurement of the lubricant level in the gear case, and a
better lubricant film in the presence of water. Field tests on the gear oils to date
indicate a very low rate of wear as compared to conventional lubricants on this large
railroad.
SWANSON's2 reported on traction-motor greases and gear lubrication on a large
railroad whose operations are discussed in historical detail. This line has had extensive
experience with various types of traction-motor gear lubricants, ranging from the
asphaltic high-viscosity types, which are still used in certain main-line applications,
and some of the soap-thickened types (not further identified). The author believes
that a heavy thickened oil fortified with proper e.p. additives might prove better than
present materials. Railroad traction-motor gear operation is considered much more
severe than industrial gear applications which occur in machinery rigidly fixed or
sohdly mounted, and even huge off-the-road tractors have large rubber tires; these
factors minimize vibration and shock. Railroad operation has longitudinal, transverse
and vertical shock forces which give much greater severity to operation because of
shock loads, vibration, and twisting on unsprung masses of traction motors, gears
and associated equipment. This mandates that all gear cases must be reasonably tight
before a thickened oil material can be successfully used as a lubricant.
Aerospace
LEWIS, MURRAY, PETERSON AND ESTEN~~~J presented a paper in 1962 on
WcX%',
16 (1970) 87-142
lubricant evaluation for bearing systems operating in spatial environments, presenting
a general summary of several programs aimed for the selection of lubricants for
rolling contact bearings. In an extensive program, seventeen greases were given a
preliminary screening, these being petroleum (soap- and non-soap-thickened)
synthetic hydrocarbons, esters, silicone-ester blends and silicones with the latter also
being soap-thickened and non-soap-thickened. A slow-speed, light-load screening test
used a 7-mm bore ball bearing at 50-60 rev.,/min and 140-150°F. Later high-speed
grease tests were at 1800 rev./min on an K-4 bearing, at 200 g axial load and 150” and
250°F. A chlorophenylmeth~ll polysiloxane grease thickened with lithium soap, and a
paraffinic petroleum oil thickened with sodium soap were found best. Barrier films
studied to prevent loss of oily fluid by “wetting” of the shield surfaces gave a large
improvement. In a separate study the combined use of radiation at 108 rads and a
vacuum showed no cause for concern, even when the irradiated greases were run in
open bearings at ~50~--~5o“F’.Discussion by Burton dealt with techniques of measuring
and interpreting vacuum tests, and Young discussed the need for lligI~er-radiation-
level studies on greases. The authors agreed, in the main, with the discussions, and
contributed further comments.
FLEMING~*~in a 1964 publication reported on the past, present and future of
space activities, describing NASA* facilities and programs. In view of the 1969
accomplishment, it is interesting to look back and see what happened in r964-man
had flown in space, unmanned explorations had been made of the moon and Venus,
weather satellites had produced valuable data, and satellites for intercontinental
radio and TV had been achieved. This paper described plans for extending the fore-
going probes and satellites and accurately predicted Apollo II mission which landed
two men on the moon in 1969, with cameras and other instruments which were left
on the moon. Plans for planetary exploration missions were also discussed.
SCHWENKER~*~ discussed grease lubricants and their potential in 1964 aero-
space applications. The scope of aerospace greases included applications on aircraft
from endurance types to the supersonic type and various missiles including the ICBM.
Space-vehicle requirements are also considered. The various properties of greases
needed to lubricate these extreme-environment mechanisms are discussed including
a list of component mechanisms in which the greases will be used. Emphasis is put on
using conventional greases where possible even though achieved only by special
design to protect them from temperature extremes, excessive radiation and hard
vacuum conditions. Descriptions are given of mineral oil and synthetic hydrocarbon
greases, ester base greases, silicone greases, gasoline- and oil-resistant types, non-
elastomer-swell types and also experimental greases using non-soap thickeners such
as the triazines, arylureas, imides and PTFE-tl~ickened fluorinated polymers. This
paper and others covered in this review bring out the long-range planning and
development given to space lubricants which may seem strictly experimental and
exotic when first developed, but which later become familiar and very useful.
JOHNSONAND RwCKLEYls9 also reported in 1964 on lubricants and mechanical
components for space environments (published in 1966). A primary problem in
producing satisfactory systems is that of selecting designs and lubricating materials
resisting evaporation and dissociation at low pressures, and at the same time giving
adequate lubrication. Frictional heat should be dissipated from devices operating in
* National Aeronautics and Space Administration.
vacuum ; a function of design which should also include minimizing heat generation.
Evaporation at low pressures is a limiting factor for greases and oils but molecular-
flow seals can extend their usefulness. Solid-film lubricants such as MO& or PTFE are
useful in thin films or solid-compact materials and resist vacuum effects. Normal
oxide films, worn away in vacuum and not replenished because of lack of oxygen,
leave the surfaces subject to catastrophic welding. Inclusions of oxides or sulfides in
alloys help replace surface films worn away and reduce failure tendencies; also,
hexagonal crystal structure helps bearing alloys to obtain low friction and minimal
wear. The paper ends with the summarized results of a questionnaire of 33 questions
sent to 50 organizations on the determination of vacuum evaporation characteristics
for lubricants.
YOUNG, CLAUSSAND DRAKE190 have considered in extensive detail the lubri-
cation of instrument ball bearings for satellite and space probe applications. This
1963 publication informs that, at that time, bearings could operate for over one year
at ro-7-10-g torr including lightly loaded grease-lubricated bearings run in small test
motors. The best grease tested in ZMCZSO lasted 9613 h at 175°F before failure, this
being a chlorophenyl methyl polysiloxane thickened with lithium soap. Dry-film
lubricants and special retainer materials were also evaluated. Discussions by Godfrey,
Furby, Jackson and Johnsonraisednumerous questions a~dcommented on details of the
testing which were answered by the authors who also presented additional data.
YOUNG AND CLAUSS~“~continued studies on lubrication for spacecraft appli-
cations. This 1966 publication reports that a chlorophenyl methyl polysiloxane
thickened with a lithium soap gives best results for operation in high vacuum (IO-~-
IO-9 torr) and temperatures up to 3oo”F, and also under radiation equivalent to one
year operation internally in orbits up to approximately zooo nautical miles (4.106 R).
Diester-base lubricants did not appear suitable for operation under vacuum. In
response to a discussion of this paper by Brown, the author wrote that lithium-soap-
base silicone grease, on the whole, seems best because of more data on this formu-
lation; however, the dye-thickened silicone grease meeting MIL-G-25013 is con-
sidered a close second. More data for statistical treatment are needed to reach firmer
conclusions.
Later experiments by CHRISTIANAND BUNTING192 at 400°F and 10-7 and
IO-~ torr have shown that special greases can successfully lubricate both small- or
large-diameter bearings under stringent speed and load conditions for very long
periods of time without relubrication. Polymeric perfluoro stocks thickened with
ammeline were the most promising products, being compatible with liquid oxygen,
stable up to 600°F at atmospheric pressure and up to 400°F at 10-7 ton (an R-4
bearing ran for 1457 h at 10-7 ton-, 400°F).
As the space program progressed, studies on lubricants became more sophisti-
cated and of greater scope. An article by DELAAT, SHELTONAND KIMZEY~~~ was
published in 1967 on the status of lubricants for manned spacecraft, primarily for
Project Apollo. Greases will be used in gear boxes and sealed bearings for the Apollo
spacecraft as well as on fittings, linkages, and other miscellaneous uses. Lithium soap
or fluorocarbon telomers are typical thickeners with base fluids being fluorocarbons,
fluorinated hydrocarbons or a silicone. Selection of lubricants including solid dry-
film types and oils was based on compatibility with oxygen-rich environment for
crew-compartment toxicity-order hazard evaluations; lub~c~t-pro~llant com-
Miscellaneous
pOPElgg discussed useful grease tests for general plant lubrication covering the
largest manufacturing plant of his company (140 major buildings, 1,000 acres,
20,000 employes). Photographic film and paper and specialty products are made here.
In production operations, temperatures range from -80 to +goo”F, speeds up to
60,000 rev./min and bearing loads from a fraction of anounce to67,ooolb. By analyzing
conditions of service, three greases have been found to satisfy all but a few special
needs: NLGI 2 sodium soap, NLGI 2 lithium soap, NLGI I calcium or aluminum
soap. Tests used to determine the suitability of greases are ASTM D 1741 Functional
Life of Ball Bearing Grease run at 125°C for sodium, barium, and complex greases
and run at IOO’C for lithium greases. Other ASTM tests are D 1743 for rust preventive
properties, D rogz for apparent viscosity, and D 1478 for low temperature torque.
The Fafnir friction-oxidation test is also used. Bushing tests varied from -2o’F to
240°F are also run to simulate service conditions. The three greases mentioned
previously are covered by specifications. Compatibility is tested by running mixtures
of pertinent greases in the ASTM D 1741 functional life test. 2,030 h in the D 1741
test is considered the minimum to select a grease for further field testing.
MOODIE~OO points out the advantages of preventive maintenance in giving
RECENT USAPUBLICATIONS ON LUBRICATINGGREASE 129
longer equipment life, better availability, and lower cost by using planned and
scheduled programs for the maintenance, adjustment, repair and lubrication of
machinery and equipment trucks in the construction industry. Eq~pment manufac-
turer’s lubrication specifications are used as guides ins electing the products (no specific
data on greases.)
KITCHEN~~~ has studied the lubrication of small motor bearings for unattended
service in automatic electromechanical telephone system equipment. Bearing
temperatures substantially exceed zoooF, and normal life expectancy based on
lubrication by conventional lubricants is about S,OOO-12,000h. In an effort to reach
IOC,OOO h or IO years of life, tests were first run in a multispeed bearing test machine.
In order to establish a reference point, a paste of a high concentration of MO&
powder in a mineral-oil-lithium-soap grease, specifically not recommended for use in
anti-friction bearings, was evaluated in bearings with no shields. It was unexpectedly
found that the bearings reached a surprisingly high projected wear life of xoo,ooo h
of operation without significant increase in tolerances, whereas with shields in place
and the same lubricant, a projected wear life of only 1000 h was obtained. The author
thinks that the bearings run with no shields permitted an escape route for agglomer-
ates of the solid-film lubricant. It was also found in motor environmental tests, that
this MoSa paste could be used in a damp environment where the externals of the
motors corroded badly but the bearings were well-protected under 60-rooo/;, relative
humidity for over 4,000 h. Discussor Vest asked how the projected wear life was
determined; the author stating that such was obtained from the motor manufacturers’
data on bearing failures at similar conditions, and the accelerated wear-test results
were treated with a factor of 70 with a reliability estimated about *zoo/b. In answer
to another question, the author stated that work was being done with formulations
that will not agglomerate so that shields can be used to retain the desirable features
of this design.
FITZSIMMONS, MURPHY, ROMANS ANDSINGLETERRY~~~ have developed barrier
films to increase the service lives of pre-lubricated miniature ball bearings used in
synchros and servomotors, these being important components of computers, guidance
controls, navigation instruments, and fire-control systems where reliable performance
of the bearings is imperative. Loss of lubricant by creeping or spreading rather than
by evaporation was found the predominating cause of short lubricating lives. Un-
acceptable lubricant loss during storage exceeding six months was found. Lubricant
loss by spreading can be prevented by coating the bearing faces with a non-wettable
fluorinated polymer, specifically the polymethacrylate ester of rH, IH-pentadeca-
fluoro-x-octanol. The barrier film also allowed more oil to be held within the bearing
which, of course, increased the operating lives. This is also true for the instrument
greases studied. However, oil is preferred for small synchros as grease-lubricated
precision bearings may have too high friction torque at low temperatures and soap
aggregates may give problems with miniature ball bearings. Liquid ester-type lubri-
cants are preferred over silicones for temperatures up to 175°C in synchros and servos
because of better lubricity and the incidence of gelatinous material in the bearings of
the new or stored units lubricated with silicones. Bearings treated with the barrier
film have increased the lives of synchros from 300 to nearly 4,000 h, and comparably
for servo motors.
The lubrication of nuclear power plants has become of pronounced interest
* Published in 1969.
sive TFPM lubricants. The authors stated that TFPM lubricants resulted in the most
economical solution.
HARSACKY~~~ reported on aircraft gear lubrication in a 1963 paper, for tempera-
ture ranges of -65”F-300°F. The smaller gears in which grease is used require an
e.p. product. Greases used in airframe gearing on an Air Force Mach z jet aircraft
described at that time were the following MIL-G products: 3278A, Grease, Aircraft
and Instrument; 7118B, the e.p. version of 3278A; 21164A, synthetic grease with
molybdenum disulfide, and 27549, Grease, Heavy Load Carrying with a mean Hertz
load (load wear index) of 60. The Air Force programs at that time were aimed at long-
term-use at 600°F.
NLGI Penetration
grease grades
000 445-475
oo 400-430
0 355-385
I 310-343
2 265-295
3 220-250
4 175-205
130-160
85-I 15
The NLGI classification has now become American Standard Zrr.r3o-rg63207 and is
being considered for international standardization at this time.
MAYORAND0~0~20s have asked whether there is more to grease classification
than consistency. An engineer designing a certain mechanism, but unfamiliar with
lubricating greases, finds nothing in the literature corresponding to the ASTM engine
test sequences, and therefore establishes a specification based on a particular product
which happened to work in his application. The authors propose a type classification,
giving limits for such properties as water washout resistance, extreme pressure (load-
carrying ability), consistency at operating temperatures, etc. with these to be coded.
They recognize the complexity of setting up a system like this for lubricating greases,
but think the need is evident. (Reviewer’s note: The recent revision of SAE Informa-
tion Report J3roa (see p. rrg) is a step in this direction, and ASTM Technical Division
B, Section IV Chassis Lubricants, and Technical Division G, Section III-9 Ball Joint
Tests are working to establish performance tests which will create more of the
“language” needed to help the equipment engineers pick the correct kinds of lubri-
cating greases.)
Sjwcifications
METZGER~~~described the specification of lubricants for a new 8o-in. hot strip
mill. This paper describes the process of standardization in a large steel company for
all of their plants. A section on lubricating grease describes the development of a
purchase specification covering an e.p. lithium-base grease of NLGI I consistency.
Various modifications of ASTM tests are described to supplement current ASTM
Standards. The former cover a modified Timken e.p. test, shear-stability tests with
the addition of water, a roller test including the effects of oxygen, and base oil tests
for viscosity, flash and fire.
SARGENT AKD BUNTING”~~ have covered grease specifications now and for the
future. This paper is within the frame of reference of a large aluminum corporation
covering a wide variety of operations. Twenty years ago, all antifriction bearings
were regreased monthly. Today (1968), the regreasing interval is once per year.
Older plants made wide use of grease-lubricated sleeve bearings, but today plants are
built with a few or no journal bearings unless they are largely grouped in one location
fcr servicing with a centralized grease system. Grease consumption has dropped from
about 400,000 lb. to about 241,500 lb. Some 90-957; of the grease volume is purchased
to one multipurpose specification. Specifications for a multipurpose product should be
based on functional tests, be reasonable, pertinent, current and use standardized
recognized tests as far as possible, such as ASTM Methods. They should also define
desired consistency or pumpability, mechanical stability, thermal stability, water
resistance, and corrosion prevention. Future specification requirements for greases
will stress thermal and mechanical stability and long-time usage. Wasteful grease
applications will decrease and quality demands will increase and a higher unit price
will be paid.
0~~211 reported on lubrication for machine tool builders in 1963 stressing that
standards and specifications are essential in developing a mutual understanding be-
tween builder and purchaser. Better manpower utilization and reduced lubricant
consumption has resulted from minimizing lubrication points by use of automatic
lubrication systems. A number of illustrated examples is given. Greases should be
specified by NLGI Grade No, and additional test characteristics rather than by brand
name.
Regulations
DOOLEY~~~ reported in 1966 on lubricants in the food industry. This paper
describes the food additive regulations of the Food and Drug Administration (FDA),
the Meat Inspection Division (MID) and the Inspection Branch of the Poultry
wear, 16 (1970)87-142
RECENT USA PUBLICATIONS ON LUBRICATING GREASE I33
Division, describing the circumstances under which lubricants become food additives.
Specifications on the various petroleum products permitted, and the limitations on
their use are given. Considerable clarification has been brought about during the
period 1960-66. Lithium-soap greases can now be used in departments where edible
products are not processed or handled, this being a relaxation of an earlier ruling of
the Meat Inspection Division. Lubricants become food additives when they have
incidental, not accidental, contact with food. When certain potential hazards are
known to the supplier, he should not recommend certain types of grease or other
lubricants to food processors in order to prevent any possible undesirable effects of
accidental contamination. A summary of specific uses of petroleum fractions and
some related substances listed in the Food Additive Regulations as of August 15,
1966 is given.
Recommended jwactices
One of the activities of the NLGI technical committee is to develop re-
commended practices for such items as grease dispensing, wheel bearing packing, ball
joint servicing, and the like. The latest practice to be announced119 is that the cubic
inch be used as a unit of measurement followed by the equivalent cubic centimeter in
parentheses as an option. This was done in connection with the standardization on a
unit of measurement for capacity ratings for dispensing equipment.
The papers covered in this last section are listed as representing a significant
portion of papers given at the NLGI meetings since 1963 and are of great importance
to those segments of the lubricat~g grease industry with which they are concerned.
Production swveys
HAGSTROM~~~ and JOHNSON AND HAGSTROM~~~, have forecasted the US
grease market from 1962 to 1975 in two papers. A slight trend to a declining volume
is noted and is forecast through x975_ However, for practical purposes, the volume
may be considered as constant. Quality requirements, and thus the prices of grease,
are escalating and continued research is needed to develop the long-life greases being
demanded. Since 1957, sodium-soap greases have declined from 22% of total produc-
tion to 13% in 1965 and simultaneously lithium-soap greases have increased from
28% to 42% of the total.
ELLIOT~~~,OSWALT~~~, and LANE~~~ have successively reported on the NLGI
annual production survey which was started in 1957. This is one of the most important
activities of NLGI, indicating, as it does, the growth of the lubricating grease industry
and also the proportion of the different kinds of greases made. There was a total of
569,038,ooo lb. of grease reported in 1966 against 503,028,000 lb. in r965.This survey
also includes data from Canada which shows 32,536,ooo lb. for 1966 against 34,973,ooo
lb. for 1965. The survey has now been put on a biannual basis.
Market&g
VESPER~~~ asked for a return to sound, fundamental selling practices for
lubricating grease products with new emphasis on improved and basic sales techniques,
Miscellaneozts
The NL,GI Spokesmalz for August 1965 (p. 137) discusses the Service Industries
activity226 of NLGI. This is a group of Associate, Marketing and Technical members
who are charged with developing effective meetings, panel discussions and publications
directed to processes, raw materials, equipment and containers pertaining to lubri-
cating greases.
HoGAN~~~ considers how to read an industrial advertisement.
ACKNOWLEDGMENT
The author wishes to thank E. J. BECKETT for preparing the References section,
and SUZANNE FREEBORN for transcribing the tapes and typing the manuscript.
REFERENCES
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2 B. W. HOTTEN, in Advances in Petroleum Chemistry alzd Refinilzg, J. J. MCKETTA, Jr. (Ed.),
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MCKETTA, Jr. (Ed.), Vol. VI, Interscience, New York, 1962, Chap. 5.
4 T. W. MARTINEK AND D. L. KLASS, Theory for inorganic-thickened grease structure, NLG1
Spokesman, 29 (Oct.) (1965) 219.
5 T. W. MARTINEK, R. M. HAINES AND D. L. KLASS, Theory for inorganic-thickened grease
structure, Part II. Electrical properties, NLGI Spokesman, 30 (Nov.) (1966) 286.
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structure. Part III. Apparatus and methods of measurement, NLGI Spokesman, 30 (Jan.)
(1967) 361.
7 G. S. BRIGHT, The use of electrical measurements as an aid in the understanding of fundamen-
tal grease structure, NLGI Spokesman, 30 C June) (1966) 84.
8 G. S. BRIGHT, Grease transitions-correlation of electrical and viscometric measurements,
NLGISpokesman. 31 (Jan.) (1968) 362.
9 E. L. ARMSTRONG, Review and appraisal of NLGI research fellowship activities, NLGI
S#okesman, 28 (Sept.) (1964) 168.
IO M. H. MILES, D. W. MILES, A. F. GABYRSH AND H. EYRING, Stress-relaxation and recovery
time for grease and polymer systems. Determination of the relaxation time parameter B,
NLG1Spokesmalz, 28 (Sept.) (1964) 172.
II M. J. VOLD AND R. D. VOLD, Progress report on the NLGI Fellowship at the University of
Southern California, NLGI Sfokesman, 29 (May) (1965) 54.
12 C. A. J. LANGMAN, M. J. VOLD AND R. D. VOLD, The effect of the liquid component on the
penetration of lithium stearate greases, NLGI Spokesman, 3r (Aug.) (1967) 152.
13 M. J. VOLD, Y. Uzu AND R. F. BILS, New insight into the relationship between phase be-
havior, colloidal structure and some of the rheological properties of lithium stearate greases,
NLGI Spokesman, 32 (Jan.) (rg6g) 362.
14 Report by Section IV, Technical Committee G, ASTM Committee D-2, Chairman H. A.
WOODS, et al., Viscosity of lubricating grease at elevated temperatures, NLGI Sfiokesman, 29
(Aug.) (1965) 146.
15 A. W. SISKO AND L. C. BRUNSTRUM, Permeability of lubricating greases, NLGI Spokesman,
25 (June) (1961) 72.
16 W. J. EWBANK, J. DYE, J. GARGARO, K. DOKE AND J. BEATTIE, Permeability coefficients as
a measure of the structure of lubricating grease, NLGI Spokesman, 27 (June) (1963) 75.
17 W. L. BROWN AND W. J. EWBANK, The effects of thickener concentration on the permeability
of lubricating grease, NLGI Spokesman, 29 (June) (1965) 77.
18 J. L. ZAKIN AND E. H. Tu, Effect of variations in the viscosity and type of mineral oil
component on the permeability coefficients of lithium-calcium and Baragel greases, NLGI
Spokesman, 29 (Jan.) (1966) 333.
rg J. L. ZAKIN AND H. H. LIN, Permeability of silica greases, NLGI Sfiokesman, 30 (Oct.)
(1966) 244.
20 W. J. EWBANK, The present status of NLGI work on permeability of lubricating grease,
NLGI Qokesman, 30 (Aug.) (1966) 167.
148 J. MESSI~A, Greases nonreactive with missile fuels and oxidizers, A\FI_GI.‘j@kesma~z, 27
(Sept.) (1963) 177.
149 J. MESSINA, An exploratory study on ~ol~~etrafluorethylene-thickened greases, P~+P&
*QSLE A anuaE ~~~~~~~~ May 5-g / 1969.
150 A. A. SCHWARTZ, Effect of penetration and thickener content on ball bearing grease perfor-
mance, Lubrication Elzg., 18 (&lay) (1962) 237. (Discussed by J, W. JOHNSON.)
151 J. I.,. DREHER, W. L. SMITHSON AND C. F. CARTER, A special grease for the food industry,
lVLG1 S$okesman, 30 (July) (1966) 126.
152 H. R. BAKER AND K. N. BOLSTER, The effect of thickener purity on the water resistance of a
semi-fluid weapons lubricant, i”rrLG1SpokosmaTa. 31 (Oct.) (1967) 249.
753 J. M. BISH, The effect of acidity and basicity of lubricating greases upon their performance,
~~G~S~~kesrnu~, 32 (Sept.) (1968) 193.
154 R. I-f. NEWMAN AND R. P. LANGSTON, The performance of calcium hydroxystearate greases
in wet conditions, NLGI .S$okesman, 30 (Aug.) (1966) 153.
155 S. F. CALHOUN AND R. L. YOUNG, Rust preventive abilities of grease and their improvement,
Lubvicafion Exg., 19 (July) (1963) 292.
156 E. I.. ARMSTRONGAND M. A. LINDEMAN, Effects of oil viscosity and soap type on torque in a
grease-lubricated journal bearing, NLGI Spokesman, 33 (Aug.) (1969) 152.
‘57 C. H. MITCHELL AND G. A. SHORTEN, The development of a muIti-pu~ose lubricating grease,
NLGI ~~~okesrn~~, 33 (Sept.) (1969) 196.
158 H. ELDRIDGE, Lubrication requirements of rg64 cars, NLGI Sfiokesmalz, 27 {Nov.) (1963) 254.
I59 H. ELDRIDGE, Lubrication requirements of 1965 cars, NLGI Spokesman, 28 (Nov.) (1964) 261.
160 H. ELDRIDGE, Lubrication requirements of 1966 cars, NLGl Spokesman, 29 (Nov.) (1965) 260.
161 H. ELDRIDGE, Lubrication of 1967 cars, *VLGI Spokesman, 30 (Dec.) (1966) 328.
162 H. ELDRIDGE, Lubrication of 1968 cars, NLGI S+okesman, gr (Dec.) (1967) 332.
163 H. ELDRIDGE, Lubrication of 1969 cars, NLGI Qokesman, 32 (Dec.) (1968) 34.2.
164 J. W. LANE AND C. F. FOELL, Let’s probe the idea of extended car service, ,%rX_GI S~~kesrn~n,
27 (April) (1963) 23.
165 SAE Information Report J-31oa, Automotive lubricating greases, IVLGI S$okesmam, 32
(April) (1968) 22.
166 D. F. MILLER, Chrysler viewpoint-lubrication, 1965 NLGI Spokesman, 28 (Dec.) (1964) 294.
167 L. F. H~YER, Arresting fleet corrosion, NLGI Sfiokesman, 26 (March) (1963) 383.
168 L. F. WAVER. The most important preventive maintenance in motor equipment care, NLGI
Spokesmaa, 29 (May) (x965) 57.
169 R. R. TISDALL, Application of corrosion preventive compounds to automobile underbodies,
~~G~S~o~e~rna~z, 26 (Jan.) (1963) 318.
‘70 E. G. WICKLATZ, New concept of protective coating application, NLGI Spokesman, 27 (Oct.)
(1963) 222.
‘7’ L. D. DROMGOLD, W. HART AND C. E. HULME, Automotive vehicle corrosion prevention
undercoating, NLGISfiokesman, 28 (May) (1964) 42.
‘72 W. A. HIGGINS, Automotive rustproofing compounds, NLGI Spokesman, 29 (March) (1966)
381.
‘73 W, G. KAUTZ, Antirust: undercoat - don‘t undercut, XLGI S~okesmu~, 26 (Jan.) (1963) 324.
174 S. F. CALHOUN, Current policies and trends in the lubrication of army equipment, NLGI
Sfvkesman, 27 (Dec.) (1963) 298.
175 J. MESSINA, L. F. PEALE, H. GISSER AND K. R. FRISCH, Lubricants for rapid-fire automatic
weapons, NLGI Sfiokesman, 28 (June) (1964) 70.
176 T. MESSINA. Perfluorinated lubricants for liquid-fueled rocket motor systems, &&ication
hzg., 23 (Nov.) (1967) 459.
177 N. D. REBUCK. L. STALLINGS AND M. I. DEVINE, New lubrication vehicle for naval aircraft,
hTLGI S~~kes~~~~, 32 (Feb.) (rg6g) 396.”
178 E. C. KRUEGER AND I’. B. LOCKWOOD, Urban transit lubrication panorama, NLGI S~~kesrna~~,
28 (March) (1965) 371,
I 7g J. B. DRIVER, Lubrication of airbrake equipment on railroad freight cars, Lubrication Eng.,
20 (Jan.) (1964) 16.
180 H. H. KOCI AND P. R. BEN, Design, operation and lubrication of traction motor gears and
gear cases, Lubrication E+ag., 24 (Dec.) (1968) 565.
181 R. R. POOLER, A new look at traction motor gear lubricants, Prep&t ASLE Annwal IMeetimg
May 9 I 1968.
182 R. F. SWANSON, Traction motor grease or gear lubrication in use on the New York Central,
Pre@ilzt ASLE Annual Meeting, May 9,1968.
183 I. R. SLINGERLAND ANII A. J. MILLER, Significance of tests of lubricating greases from the
standpoint of an agricultural marketer, NLGI S+okesman, 27 (Jan.) (x964) 327.
184 C. X. HINKLE, Lubricating farm machinery, NLGI S#okesman, 29 (June) (1965) 89.
~17 J. 1%‘.LANE, NLGI’s annual production survey, A’LGI Sfiokesma?~., 31 (Aug.) (rgb7) IO_+.
218 H. G. VESPER, Have we forgotten how to sell?, NI*GI Spokesman, zy (Dec.) (1965) ~95.
219 L. 11. OFFER, Marketing automotive undercoats, NLGI Spokesman, 27 (Jan.) (1964) 3~ 7.
220 11. Ii. FHRMACHER, One way to combat the present unsatisfactory profit trend in the farm
market, NLGI Spokesma?z, 27 (July) (1963) 112.
221 C. E. GORE, Iiustproofing: Opportunity for new profits, *VLGI S~okesma~z, 28 (April) (1964) 8.
222 C. I<. GORE, We have to market if we arc going to sell, NLGI Spokesma~~, 30 (Sept.) (1966)
198.
223 H. J, SIEGLE, The market for industrial oil and grease in the manufacturing industries, NLGl
Spokesman, 31 (Feb.) (1968) 389.
224 F. J. MENTOX, To buy or not to buy that is the question, 9LGI Spokesman, 32 (Jan.) (1969)
374.
225 J. E. MAHONEY AND T. J. KOON, A marketing viewpoint of coal mine lubrication, &VTLGI
Spokesman, 33 (May) (1969) 47.
226 Anon., Service industries activity of NLGI, NLGZ Sfiokesman, 29 (Aug.) (1965) 137.
227 W. T. HOGAN, How to read an industrial ad., NLGI Spokesman, 32 (July) (1968) I 28.
Wear, 16 (1970);87-142