Journal of ASTM International, Vol. 6, No.

1
Paper ID JAI101691
Available online at www.astm.org

R. A. Kishore Nadkarni1

Engine Oil Volatility: Noack Evaporation Methods

ABSTRACT: The Noack evaporation loss is an important test for base oils and lubricating oils used in
internal combustion engines. The alternate test methods used for this determination are described and
evaluated regarding their applicability in the field.
KEYWORDS: Noack volatility, evaporation loss, lubricating oils, engine oils

Introduction
Evaporation loss is a critical parameter of interest to automotive manufacturers, and it is included in
several oil lubricant specifications. Evaporation may contribute to oil consumption in an engine and can
lead to a change to the properties of an oil. The loss of volatile materials can adversely affect the original
performance characteristics of a lubricant and therefore could be a significant factor in evaluating a
lubricant for a specific use. Such volatiles can become contaminants in the environment in which the
lubricant is to be used. Originally in Europe and later in North America and Japan some years back,
maximum volatility limits were included in the crankcase lubricant specifications. Since the volatility
limits may have a significant impact on the formulation and ultimate production costs, this necessitated the
development of volatility test with acceptable precision limits. There are a number of engine oil volatility
tests based on diverse techniques such as gas chromatography-distillation ASTM D5480, D2887, etc. or
physical measurements thermogravimetric analysis ASTM D6375 and Noack evaporation test ASTM
D5800.
Gas chromatographic GC methods are widely used in the analytical laboratories for a variety of
organic analysis. Among these are ASTM D2887 for boiling range distribution of petroleum fractions, and
D5480 for engine oil volatility. The former was specified by the automotive industry to measure oil
volatility. The method in D2887 does not have very good precise volatility and is limited to oils that have
a final boiling point 1000 F. As an improvement over ASTM D2887, McCann et al. devised a modification using high temperature capillary GC procedure using an internal standard. The procedure could
obtain a precision of 12 % RSD 1. However, the GC methods do not necessarily duplicate the engine
conditions that contribute to lubricant volatility, and necessitate the use of an arbitrarily chosen volatility
temperature and the use of an internal standard to correlate with overall losses during distillation.
The Noack volatility test which evolved was ultimately accepted by both the oil and automotive
industries and is today considered a vitally important test in the characterization of lubricating oils and
base oils. This test method is based on the principle of loss of mass at a constant temperature under a
constant stream of air, a principle developed by Dr. K. Noack in Germany in 1930s 2. The original Noack
method was designated as DIN 51-581, and later was documented by CEC as L-40-A93, by ASTM
International as D5800, by IP now EI as IP 421, and in Japan as JPI 55-41-93. The ASTM method was
later modified to include procedures A, B, and C. In all these methods, the evaporation loss is defined as
that mass of oil lost when the sample is heated in a test crucible through which a constant flow of air is
drawn. A low Noack value indicates an oil that will maintain its original protective performance qualities
for a longer period of use. In all Noack procedures, the precision and accuracy of the results are dependent
on a mandatory use of a certified reference standard for the verification of the instrument operation. The
equipment needs to be referenced approximately every ten tests if the test is used frequently. If the testing
is infrequent, the equipment should be referenced before the first sample of the day is run. If the percent
Manuscript received January 31, 2008; accepted for publication November 10, 2008; published online December 2008.
1
Millennium Analytics, Inc., East Brunswick, NJ 08816.
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evaporation loss of the reference fluid is not within the limits given, the instrument should be checked for
operating precision or recalibrated before samples are tested. Often CEC reference oil RL-172, RL-223/3,
or other equivalent fluid is used as the reference fluid. This oil can also be utilized as a quality control
sample for statistical quality assurance of the instrument performance.
Test Method ASTM D5800 Procedure A
In this as well as in its equivalent DIN 51-581 and CEC L 40-A93 methods, a measured amount of the
sample is placed in an evaporating crucible which is then heated to 250 C with a constant flow of air
drawn through it for 60 min. The loss in the mass of the oil is then determined. The method uses Woods
metal as a heating medium. Safety Considerations. There are two safety concerns in utilizing the above
procedure A method: volatilization of the heated oil, and release of toxic metals from the Woods metal
heating block at 250 C during testing. Woods metal is made up of lead 25 %, tin 12.5 %, bismuth
50 %, and cadmium 12.5 %, all toxic materials and chronic poisons. Although the method calls for
operation in a draft-free area, the exhaust fumes from the evaporating oil must be ventilated to an outside
source. Thus, the analyzers must be operated in well-ventilated hoods. Further specific precautions may be
necessary to prevent exposure to these toxic metal fumes and heated oil vapors. At least two vendors are
selling instruments procedures B and C which do not use Woods metal as a heating medium.
A second concern is the exposure to heated oil fumes in the vicinity of the apparatus. Although the test
method calls for a draft-free area, the exhaust fumes from the evaporating oil must be ventilated to an
outside source. For safety reasons, some laboratories place the Noack apparatus in a hood. Others place it
on a bench-top with an elephant trunk to draw the fumes. Higher volatility results have been observed
when the apparatus is used in a hood, because the airflow will sweep the fumes from the top of the
crucible. ExxonMobil Research and Engineering Company proposed a shield for creating a draft-free
environment and greater safety in operation 3. This device isolates the instruments heater block environment using a metal box, thus greatly reducing the air flow immediately around the sample while
allowing sufficient thermal exchange. The accessory can be made from a 14GA aluminum sheet for a box
fitted to the top of the heating block with its length and width somewhat larger than the dimensions of the
top of the heating block. The box has slots in the sides to allow for protruding outlet tubes and temperature
sensor wires and a hole in the top to allow heat escape. This device is described in Appendix X3 of
D5800-05 standard, and is now commercially available from the vendor ISL. The use of this draft deflector
significantly improves the accuracy and the precision of Noack testing as shown by ExxonMobil 3.
Given overall safety concerns and the declining use of this particular instrument, CEC has deleted this
procedure from its L-40 standard as of 2007. However, it remains as procedure A in the ASTM D5800
standard.
Test Method ASTM D5800 Procedure B
An alternative to the use of Woods metal as a heating medium was developed by French instrument
manufacturer ISL later part of PAC Instruments in 1998. The method uses the same principle and the
same crucible of the original Noack test method, but does not use the Woods metal as a heating medium,
and the sample temperature is directly monitored. At present, this is probably the most widely used
technique for Noack volatility measurements.
Test Method ASTM D5800 Procedure C
A second alternative to using Woods metal heating medium was developed by Savant Laboratories, Inc.
It uses the so-called Selby-Noack volatility test equipment and uses a special noble metal sheathing
bonded to the volatility chamber. It relates to one set of operating conditions, but may be readily adapted
to other conditions when required. The Selby-Noack procedure correlates well with the Noack procedure
A. Since then the Selby-Noack procedure has been modified to also run procedure B. The data showed no
significant bias against the procedure B results.
The instrument also permits collection of the volatile oil vapors for the determination of their physical
and chemical properties, by using a specially designed coalescing system placed just ahead of the collecCopyright by ASTM Int'l (all rights reserved); Thu Sep 2 14:20:45 EDT 2010
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NADKARNI ON ENGINE OIL VOLATILITY 3

TABLE 1Precision of noack volatility test methods.
Procedure
CEC L40-A93
ASTM D5800 A
ASTM D5800 B
ASTM D5800 C
ASTM D6375

Repeatability
0.18+ 0.031 X
5.8 % X
0.095 X0.5
0.81 %
0.31 X0.60

Reproducibility
0.40+ 0.069 X
18.3 % X
0.26 X0.5
1.62 %
0.39 X0.60

X is the m % evaporation loss.

tion flask which is cooled in dry ice. At all levels of volatilization the recovery is essentially complete
about 99.5 %. The details of the early development of this technique can be found in several publications
by Selby et al. 47. Elemental analysis of the collected volatiles may be helpful in identifying components such as phosphorus, which has been linked to premature degradation of the automotive emission
system catalysts. It appears that some phosphorus compounds in the fresh engine oils decompose and are
found in the volatiles. The amount of phosphorus in the volatiles is independent of the volume of the
volatile products. Selby coined a term Phosphorus Emission Index to quantify the amount of volatile
phosphorus species released during the Noack-Selby test 8. He has shown that the phosphorus volatility
is not related to engine oil volatility or to the phosphorus content of the oil. This lack of correlation could
be due to the effects of other engine oil additives and/or variations in the phosphorus additive chemistry.
Marked differences were found depending on whether primary or secondary alcohols were used in the
ZDDP.
Using 31P NMR technique, different oils formulated with different ZDDPs and other additives were
found to have different volatile components. The composition of the volatile phosphorus containing components depended on the specific ZDDP 9.
Test Method ASTM D637505
As an easier alternative to the Noack method, Ford Motor Company researchers developed a thermogravimetric TGA method which was faster, safer, and employed no hazardous chemicals 10. Rico de Paz of
Texaco developed the crosscheck based on above TGA principle which resulted in the ASTM D6375 test
method 11. This method is also equivalent to EI methods IP 393 and IP 418. The TGA method is
applicable to base stocks and fully formulated lubricating oils having a Noack evaporative loss from
0 to 30 m %. The procedure requires much smaller size sample than in the Noack procedure. A lubricant
sample is placed in an appropriate TGA specimen pan that is placed on the TGS pan holder and quickly
heated to between 247 C and 249 C under a stream of air, and then held isothermal for an appropriate
time. Throughout the process, the TGA monitors and records the mass loss experienced by the specimen
due to evaporation. The Noack evaporation loss is subsequently determined from the specimens TG curve
versus the Noack reference time determined under the same TGA conditions.
Noack Test Methods Precision
Table 1 summarizes the precision obtained in the interlaboratory studies for the five main Noack tests. This
precision obtained in the original crosschecks is also borne out by the continuing Interlaboratory Crosscheck Proficiency programs conducted by D02.CS 92 as shown in Table 2 comprising of lube oil and base
oil data from the cross checks conducted in 2002 through 2007.
Test Method Biases
On an absolute basis there is no bias for the Noack methods since it is an empirical method and there are
no certified standard reference materials available. However, there are subtle differences between the
alternate approaches to the Noack evaporation determination procedures, in spite of apparent agreement
between the results by three procedures shown in Table 2. The Noack values in Table 2 cover a wide range
of Noack values each with its own reproducibility that can mask any differences; higher repeatability for
procedure C is in part because of fewer laboratories making the analyses. To determine the differences
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TABLE 2Comparative Analysis of Oils by Alternative Noack Procedures.
Sample
Lube oils
LU 0201
LU 0205
LU 0209
LU 0301
LU 0305
LU 0309
LU 0401
LU 0405
LU 0409
LU 0505
LU 0509
LU 0601
LU 0605
LU 0609
LU 0701
LU 0705
LU 0709
LU 0801
LU 0805
LU 0809
Base oils
BO 0206
BO 0212
BO 0312
BO 0406
BO 0412
BO 0506
BO 0512
BO 0606
BO 0612
BO 0704
BO 0708
BO 0712
BO 0804
BO 0808

D 5800 A

D 5800 B

D 5800 C

7.63 0.38 20
22.32 1.39 24
14.54 0.95 22
14.77 0.63 20
14.92 0.74 21
12.60 0.59 20
13.84 0.97 21
16.02 1.28 19
12.12 0.56 19
10.69 0.59 19
14.61 0.77 24
9.51 0.53 19
14.20 0.89 15
13.87 0.71 19
6.40 0.58 15
13.85 1.58 16
10.83 0.46 15
13.42 0.91 16
9.94 0.86 18
10.18 0.50 14

7.74 0.26 17
23.06 0.71 19
14.78 0.50 19
15.05 0.41 18
15.31 0.54 21
12.83 0.30 22
14.04 0.55 23
16.35 0.42 26
12.57 0.25 19
11.21 0.54 35
14.55 0.56 33
10.10 0.34 31
14.60 0.57 39
14.50 0.54 36
6.66 0.21 36
14.49 0.58 32
10.81 0.33 34
13.93 0.61 27
10.36 0.26 30
10.34 0.32 33

7.46 0.78 5
23.85 2.44 4
14.78 0.25 4
15.30 0.34 3
14.25 1.43 3
12.43 0.34 4
13.57 0.49 4
16.85 1.17 4
12.60 0.21 4
10.99 0.95 7
14.54 0.95 5
10.68 0.53 5
14.83 0.65 4
14.29 0.34 5
6.40 0.32 4
13.72 1.43 5
11.10 0.83 5
14.30 0.32 2
10.34 1.40 5
10.05 0.54 4

27.60 3.43 7
24.08 1.81 6
26.44 1.35 7
25.93 0.82 7
2.66 0.27 8
1.05 0.14 8
5.51 0.63 5
6.76 0.27 8
16.59 0.68 6
20.28 0.51 7
19.62 1.26 8
2.56 0.15 5
14.34 0.79 8
14.22 1.02 7

27.54 0.90 9
23.96 0.46 12
25.04 0.76 13
14.91 0.38 16
2.55 0.12 16
1.04 0.14 17
5.16 0.32 18
6.75 0.40 16
16.86 0.63 13
20.04 0.72 21
19.19 1.02 19
2.54 0.12 21
14.35 0.54 20
14.14 0.39 21

14.1 1
14.63 0.58 3

between Procedures A and B, many measurements were made by a number of laboratories on the same
reference materials and thus, the difference between procedures A and B was determined.
Noack results using ASTM procedures D5800 A and B show consistent differences. Procedure A gives
slightly lower results versus procedure B on formulated engine oils, while procedure A gives higher results
versus procedure B on basestocks. Interlaboratory tests have shown that procedures A, B, and C yield
essentially equivalent results, with a correlation coefficient of R2 = 0.996 see Table 2. The data in Table
2 represent the results obtained through ASTM D02 Committees CS 92 Interlaboratory Proficiency Testing program from 2002 through 2008 conducted three times a year on a worldwide basis.
A test result obtained using one of the procedures can be transformed to an estimated result on the
basis of the other procedures as follows.
a For formulated engine oils in the volatilities range of 10.5 to 21.5 m % Noack, Result by D5800
B = 1.030 X result by D5800 A, and Result by D5800 A = 0.970 X Result by D5800 B.
The 95 % confidence limits for the regression coefficients for these equations are 1.025 to 1.036, and 0.965
to 0.976, respectively.
b For basestocks in the volatility range of 4 to 25 m % Noack, Result by D5800 B = 0.962 X Result
by D5800 A, and Result by D5800 A = 1.039 X Result by D5800 B. The 95 % confidence limits
for the regression coefficients for these equations are 0.956 to 0.969, and 1.032 to 1.046, respectively.
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NADKARNI ON ENGINE OIL VOLATILITY 5

Only if the nature of the test specimen is known with certainty, i.e., whether it is a basestock or a
formulated oil, above equations may be used to convert results on the basis of procedure A or B. If the
nature of the test specimen is not definitively known, i.e., whether it is a basestock or a formulated oil,
these conversion equations should not be used to obtain results from one procedure to the other.
Limited amount of data available shows that procedures A and C give similar results for formulated
engine oils. However, no comparative data is available for the basestocks. Further work is necessary to
quantitate the relationship.
Values in Table 2 are expressed in m % as robust mean robust standard deviation number of valid
results. For this set of base oil samples, laboratories did not submit results by procedure C. As can be seen
from this table, while the use of procedure A has remained relatively static, the use of procedure B has
significantly increased, while procedure C is used in a much smaller number of laboratories. Recently,
CEC has decided to omit procedure A from its protocol because of the hazards associated with the Woods
metal as well as declining number of labs using that procedure. Thus, at least at present procedure B seems
to be the dominant means of determining the engine volatility in automotive and oil industries.

Quality Management in Noack Analysis

Noack volatility is an empirical test. That means, per se, there is no calibration or standardization step
involved in the analysis. Hence, to obtain best accuracy and consistency of results it is important to follow
the test method instructions correctly. Additionally, special attention should be given to the following
points:
a A reference oil with certified value must be analyzed in the beginning of each test cycle. If the
percent evaporation loss is not within the limits given, the instrument should be checked for
operating parameters, and reverified with the reference fluid.
b A quality control sample representative of the samples being routinely tested should be included
in the analysis sequence. Any out of control data should trigger investigation for root causes.
c Strong air drafts or turbulence around the instrument may adversely affect the test results. The
instrument should not be placed in a draft area; however, the exhaust fumes from the evaporating oil should be ventilated to an outside source. An alternative means for preventing air drafts
described in the ASTM D5800 test method has proven effective in experience.
In summary, the ASTM D5800 Noack volatility test is an important and crucial test for characterizing
the performance of engine lubricants for both automotive and oil industries. Its importance will surely
increase with newer oil classification grades on the way, which further restrict the engine oil volatility
limits. An equally intriguing aspect is perhaps the volatility of phosphorus compounds in these oils, and
characterization of the phosphorus species present in the volatiles, which can cast light on further refining
of these products to make them less harmful to automotive engine parts such as pollution prevention
catalysts.

References
1
2
3
4

McCormack, A. J., Mc Cann, J. M., and Bohler, R. J., LC-GC, Vol. 9, No. 1, 1990, pp. 2832.
Noack, K., Angew. Chem., 1936, Vol. 49, p. 385.
DiSanto, F., Presentation at the ASTM D02 Meeting, Salt Lake City, UT, June 2004.
Selby, T. W., Reichenbach, E. A., and Hall, R. H., Proceed. 9th International Colloq. On Tribology,
1994, Esslingen, Germany Bartz, W. J., Ed., 5.5, pp. 111.
5 ibid-Amer. Chem. Soc. Publication, 1994.
6 Selby, T. W. and Reichenbach, E. A., Proceed. International Tribology Conf., Yokohoma, Japan,
1995, pp 14.
7 Cluff, B. J., McMahon, D., and Selby, T. W., SAE Technical Paper, 961227, pp. 5760.
8 Selby, T. W., Bosch, R. J., and Fee, D. C., J. ASTM Int., Vol. 2, No. 9, 2005, pp. 239254.
9 Bosch, R. J., Fee, D. C., and Selby, T. W., J. ASTM Int., Vol. 2, No. 9, 2005, pp. 255273.
10 Zinbo, M., and Skewes, L. M., Thermochim. Acta, Vol. 154, 1989, pp. 367376.
11 de Paz, E. F., and Sneyd, C. B., SAE Technical Paper 962035 1996.

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