Thermal Analysis Application No.
UC 252
Thermal Analysis Application
Application published in METTLER TOLEDO Thermal Analysis UserCom 25
Determination of the Noack evapora-
tion loss of lubricants by TGA
Abstract
For quality and environmental reasons,
lubricants for engines and other applica-
tions must only exhibit a low evaporation
rate. The loss of volatile components from
an oil increases its viscosity and leads to
increased oil consumption, coking and
wear. The Noack method is a widely used
standard test method for measuring the
evaporation loss from lubricating oils.
According to the ILSAC GF-3 and API-SL
specifications the evaporation loss must
not be greater than 15%.
The ASTM standard test method D6375
for the determination of the evapora-
tion loss of lubricating oils by the Noack
method [1] uses thermogravimetric anal-
ysis, TGA. This method yields the same
results as other standard test methods
(e.g. ASTM D5800 [2], DIN 51581-1 [3],
JPI-5S-41-93 [4]).
This article describes how the Noack
evaporation loss is determined in com-
parison to a reference oil sample using
TGA.
Introduction
The increase in the usable lifetime of
lubricants coupled with faster oil circu-
lation rates, longer oil change intervals
and lower lubricant consumption means
that lubricants are subjected to greater
stress. Higher temperatures coupled with
smaller oil volumes and higher perform-
ance lead to a constant increase in the
demands placed on the performance and
quality of the lubricants. To ensure that
the lubricants are properly used, they
must be properly specified and classified.
The specifications describe the physical
properties of engine oils such as the vis-
cosity, evaporation loss and shear stabil-
ity. Performance behavior is also tested
in engine tests. This includes wear pro-
tection and cleanliness as well as the
influence on fuel consumption and the
changes in the engine oil during opera-
tion due to viscosity changes (thicken-
ing). The classification is provided by
organizations such as ILSAC, API or SAE
(see the table of acronyms).
Acronyms
API: American Petroleum Institute
ASTM: ASTM International, originally
known as the American Society
for Testing and Materials
DIN: Deutsches Institut für Normung
(German Institute for Stand-
ardization)
ILSAC: International Lubricant Stand-
ardization and Approval
Committee
JPI: Petroleum Association of Japan
SAE: SAE International, Society of
Automotive Engineers
One of the commonly used specifications
is the evaporation loss. The low molecular
mass constituents of an engine oil, which
consists of fractions of different hydro-
carbons with different chain lengths and
molecular masses, can evaporate under
increased thermal stress. This usually
leads to an increase in the viscosity of the
lubricant. At the same time, the solubil-
ity of the additives in the base oil is af-
fected.
 The evaporation is important for all lu-
bricant groups (e.g. also for synthetic
oils) if they are used at higher tem-
peratures. For example with engine oils,
evaporation losses can occur through
Thermal Analysis Application
high temperatures at the piston rings
and elsewhere. These losses lead to un-
desirable oil thickening and increased oil
consumption.
The Noack evaporation loss
test according to ASTM D6375
The Noack test to quantitatively deter-
mine the evaporation loss of oils under
standard conditions was introduced
many years ago. For example, the
DIN 51581 [3] test method measures the
evaporation loss over a period of one hour
at 250 °C under vacuum (2 mbar).
The ASTM D6375 standard thermogravi-
metric test method was developed [5] to
combine the advantages of the gas chro-
matographic method [6] with the real-
istic conditions of the traditional Noack
test. The method is quicker and more
reliable than both and can be performed
with less sample material.
According to the ASTM D6375 method, a
sample is heated rapidly in a crucible to
249 °C and held isothermally for 30 min
at this temperature during which time
the TGA curve is recorded. The Noack
evaporation loss is the loss in mass up to
the Noack reference time.
This time is determined beforehand un-
der the same experimental conditions
with a Noack reference oil. In this meth-
od, it is important that the sample tem-
perature quickly rises to a value between
247 and 249 °C but does not overshoot.
To simulate the traditional Noack meth-
od, a sample is usually heated to 220 °C
at 100 K/min and then to 249 °C tion, the tlag parameter for this cruci-
at 10 K/min. The sample mass (m s) to
Figure 1. Determination of the evaporation loss (Noack volatility) from a synthetic engine
oil using the TGA Noack test method. Black continuous curve: reference oil; red curve: syn-
thetic 5W40 engine oil; black dashed curve: sample temperature.
be used is determined from the internal
diameter of the crucible (d) using the fol-
lowing equation:
ms = 350d3
where d is in cm and ms in mg.
Performing a Noack test
The Noack evaporation test (also referred
to as Noack volatility) was performed
under the following conditions using a
METTLER TOLEDO TGA instrument:
• Crucible: 100 µL aluminum without
lid (internal diameter 0.56 cm)
• Sample mass: 61 ± 3 mg
• Purge and protective gas:
total 80 mL/min air
• Noack reference oil: W4520001 with
10.93% mass loss up to the Noack
time; supplier: Walter Herzog GmbH
• Temperature program: 50 to 220 °C
at 100 K/min, followed by heating to
249 °C at 10 K/min and isothermal
at 249 °C. To achieve the above condi-
ble was adjusted to zero.
The sample (test oil) used was a synthetic
5W40 engine oil.
Figure 1 shows the TGA curve (black
line) of the reference oil. The Noack ref-
erence time is 17.56 min; this is the time
at which the certified loss of 10.93% is
reached (see the black arrows). The TGA
curve of the sample is shown as the red
curve. After 17.56 min the loss is read off
as 7.80% (see red arrows): the synthetic
5W40 engine oil thus has a Noack evapo-
ration loss of 7.8%. This is often given
in the oil specification simply as NOACK
7.8%.
According to ASTM D6375, the repeat-
ability with 8% loss is about 1% for two
determinations by the same laboratory,
and the reproducibility is about 1.4% for
two determinations by different labora-
tories.
According to ASTM D6375, the TGA fur-
nace must be regularly heated out. The
method recommends that this is done
after about ten determinations. The fur-
nace should be heated to 1000 °C without
METTLER TOLEDO
TA Application No. UC 252 2
 a crucible and held isothermally at this
temperature for about 5 min. The air gas
flow is left at about 80 mL/min.
Conclusions
Thermal Analysis Application
Over the past years, the demands placed
on lubricants in many application areas
have changed significantly. Thermal oxi-
dation stability, low tendency to evapo-
rate and their influence on our natural
and working environments have become
very important. The innovative devel-
opment of modern lubricants and their
proper application have far-reaching eco-
nomical consequences. Lubricants (base
liquid and additives) that have been opti-
mized for the different tasks, for example
with low evaporation losses,
Mettler-Toledo AG, Analytical
CH-8603 Schwerzenbach, Switzerland
Phone +41-44-806 77 11
Fax +41-44-806 72 60
Internet www.mt.com
Subject to technical changes
©01/2010 Mettler-Toledo AG
Marketing MatChar
• save energy
• reduce service intervals
• minimize wear
• increase engine service life
• increase oil change intervals (life-
time)
and result in considerable economi-
cal savings. The determination of the
evaporation loss by thermogravimetry
is therefore an important step in the
qualification of lubricant. The METTLER
TOLEDO TGA system with sample robot
and automated evaluation provides high
sample throughput and rapid pass/fail
assessment of the oil in question.
Literature
[1] ASTM D6375 Standard Test Method
for Evaporation Loss of Lubricating
Oils by Thermogravimetric Analyzer
www.mt.com/ta
(TGA) Noack Method.
[2] ASTM D-5800 Test Method for Evapo-
ration Loss of Lubricating Oils by the
Noack Method.
[3] DIN 51581-1, 2003-02 Determination
of the evaporative loss of petroleum
products by the Noack method – Part
1 (original in German).
[4] JPI-5S-41-93 Determination of Evap-
oration Loss of Engine Oils (Noack
Method).
[5] E. F. de Paz, C. B. Sneyd – The Ther-
mogravimetric Noack Test: a Precise,
Safe and Fast Method for Measuring
Lubricant Volatility, Subjects in Engine
Oil Rheology and Tribology, SP1209,
International Fall Fuel and Lubricants
Meeting, San Antonio 1996, available
also as SAE Technical Papers, Docu-
ment Number: 962035.
[6] DIN 51581-2, 1997-05 Determination
of the evaporation loss of petroleum
products by gas chromatography –
Part 2 (original in German).
Publishing Note:
This application has been published in
the METTLER TOLEDO Thermal Analysis
UserCom No. 25.
See www.mt.com/ta-usercoms
For more information
METTLER TOLEDO
TA Application No. UC 252 3