ASTM D6375-99a
(Test Method)Standard Test Method for Evaporation Loss of Lubricating Oils by Thermogravimetric Analyzer (TGA) Noack Method
Standard Test Method for Evaporation Loss of Lubricating Oils by Thermogravimetric Analyzer (TGA) Noack Method
SCOPE
1.1 This test method covers the procedure for determining the Noack evaporation loss of lubricating oils using a thermogravimetric analyzer test (TGA). The test method is applicable to base stocks and fully formulated lubricant oils having a Noack evaporative loss ranging from 0 to 30 weight percent. This procedure requires much smaller specimens, and is faster, easier and safer than the standard Noack methods.
1.2 The evaporative loss determined by this test method is the same as that determined using the standard Noack test methods.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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An American National Standard
Designation: D 6375 – 99a
Standard Test Method for
Evaporation Loss of Lubricating Oils by Thermogravimetric
Analyzer (TGA) Noack Method
This standard is issued under the fixed designation D 6375; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope CEC L-40-T-87 Evaporation Loss of Lubricating Oils
JPI-5S-41-93 Determination of Evaporation Loss of Engine
1.1 This test method covers the procedure for determining
Oils (Noack Method)
the Noack evaporation loss of lubricating oils using a thermo-
SAE 962035 The Thermogravimetric Noack Test: A Pre-
gravimetric analyzer test (TGA). The test method is applicable
cise, Safe and Fast Method for Measuring Lubricant
to base stocks and fully formulated lubricant oils having a
Volatility
Noack evaporative loss ranging from 0 to 30 mass %. This
IP 421 Evaporation Loss of Lubricating Oils
procedurerequiresmuchsmallerspecimens,andisfasterwhen
multiple samples are sequentially analysed, and safer than the
3. Terminology
standard Noack method using Wood’s metal.
3.1 Definitions of Terms Specific to This Standard:
1.2 The evaporative loss determined by this test method is
3.1.1 Noack reference oil—the oil provided by Noack
the same as that determined using the standard Noack test
equipment manufacturers to check proper operation of the
methods.
Noack evaporation tester.
1.3 The value stated in S.I. units are to be regarded as the
3.1.2 Noack reference time—the time (in minutes) required
standard.
for the Noack reference oil to reach its known Noack evapo-
1.4 This standard does not purport to address all of the
rative loss under the conditions used in this test method.
safety concerns, if any, associated with its use. It is the
3.1.3 TGA Noack volatility—the evaporative loss (in mass
responsibility of the user of this standard to establish appro-
percent) of a lubricant as determined in this test method.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
4.1 A lubricant specimen is placed in an appropriate TGA
2. Referenced Documents
2 specimen pan. The pan is placed on the TGA pan holder and
2.1 ASTM Standards:
quicklyheatedtobetween247and249°Cunderastreamofair,
D 5800 Test Method for Evaporation Loss of Lubricating
and then held isothermal for an appropriate time. Throughout
Oils by the Noack Method
this process, the TGA monitors and records the mass loss
E 473 Terminology Relating to Thermal Analysis
experienced by the specimen due to evaporation. The Noack
E 1582 Practice for Calibration of Temperature Scale for
evaporationlossissubsequentlydeterminedfromthespecimen
Thermogravimetry
weight percent loss versus time curve (TG curve) as the mass
2.2 Other Documents:
percent lost by the specimen at the Noack reference time
DIN 51-581 Determination of Evaporation Loss of Lubri-
3 determined under the same TGA conditions.
cating Oils
5. Significance and Use
5.1 This test method is a safe and fast alternative for
determination of the Noack evaporation loss of a lubricant.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.06 on Analysis of Lubricants.
Current edition approved June 10, 1999. Published August 1999. Originally Available from CEC, Madou Plaza, 25th floor, Place Madou, B-1210, Brussels,
published as D 6375–99. Last previous edition D 6375–99. Belgium.
2 5
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from Petroleum Assoc. of Japan, Keidanren No. 90-4, 1 Chrome,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Ohtemachi, Chiyoda-Ku, Tokyo 100-0004, Japan.
Standards volume information, refer to the standard’s Document Summary page on Available from Society of Automotive Engineers, 400 Commonwealth Drive,
the ASTM website. Warrendale, PA 15096.
3 7
Available from Deutsches Institut fur Normunge, Beuth Verlag GmbH, Burg- Available from American National Standards Institute, 11 W. 42nd St., 13th
grafenstrasse 6, 1000 Berlin 30, Germany.
floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6375 – 99a
FIG. 1 Examples Showing Adaptation of Alternative Sample Pans
5.2 The evaporation loss of a lubricant is important in the 8.2 When necessary, burn out the TGA to remove any
hot zones of equipment where evaporation of part of the
condensed liquids or deposits, which may have formed on its
lubricant may increase lubricant consumption. inside surfaces. Generally, burn out is accomplished by raising
5.3 Somelubricantspecificationsciteamaximumallowable
thetemperatureoftheTGAtoaminimumof800°Cwithanair
evaporative loss. purge from 200 to 500 mL/min, and by maintaining it at this
high temperature until no smoke is detected from the TGAgas
6. Apparatus
exhaust tube. Normally 15 to 20 min at these conditions are
enough to remove most deposits. (Caution: Do not place a
6.1 Thermogravimetric Analyzer, with the capability to
specimenpanintheTGAduringthisoperation.Itwillmeltand
meetalltheconditionsrequiredforthistestmethod,alongwith
may damage the balance or furnace mechanisms.)
the software necessary to complete the required analyses.
6.2 Aluminum Specimen Pan—Thisshallbecylindrical,and
8.3 Check operation of TGA balance and adjust when
have a minimum inside diameter/height ratio of 0.45 and a
necessary. Follow manufacturer’s procedure and recommenda-
volume of 50 6 3 µL. If the pans provided by the particular
tions.
TGA manufacturer do not meet these criteria, alternative pans
may be used and adapted to fit the pan holder of the TGA.
9. Procedure
Examples of some of the adaptations used during the evalua-
9.1 Determination of Specimen Mass:
tion of this test method are shown in Fig. 1.
9.1.1 Determine the nominal internal diameter (in centime-
6.3 Pressure Regulator, capable of maintaining air delivery
tres) of the specimen pans by measuring the internal diameter
pressure at the level required by the TGA instrument.
of10differentpansandaveragingtheresults.Acalipershallbe
6.4 Flowmeter, with a flow control valve capable of setting
used to make this measurement.
and measuring the air throughput required by the TGA instru-
ment. 9.1.2 Calculate the specimen mass using following equa-
tion:
7. Reagents and Materials
M 5 350 ~ID! (1)
s
7.1 TGA Temperature Calibration Standards—These mate-
rials will depend on the particular TGA apparatus and its
M = Specimen mass, mg (round to closest whole mg.)
capabilities. The TGA manufacturer typically provides them s
ID = Nominal inside diameter of specimen pan, cm (see
and describes their use in the operating manual for the
9.1.1).
instrument.
9.2 Air Flowrate— Set air flowrate to that recommended by
7.2 Compressed air at a pressure suitable for operation of
the TGA instrument. Reagent grade air is not necessary but the TGAmanufacturer or higher if during the initial tests with
may be used if there are concerns over possible contamination the Noack reference oil there appears to be condensation on
any part of the TGA balance mechanism or furnace lining.
of the internal parts of the TGA.
7.3 Noack Reference Oil—Oil having a known Noack Repeat 8.1 with the new flow rate.
evaporative loss, the value of which is provided by the
9.3 Temperature Program (see Note 2):
manufacturer.
NOTE 2—This section only needs to be done during the initial set up of
the method in the TGA.
8. TGA Preparation and Calibration (see Note 1)
9.3.1 Using the correlation from 8.1, determine the final
NOTE 1—This section only needs to be done if TGA has been idle for
program temperature required to obtain a final specimen
an extended period of time, has had significant repairs made to it, or has
been mishandled or its location changed.
temperature of 249°C.
8.1 Check the temperature correlation between the speci- 9.3.2 Program the TGA to heat the specimen from 50°C to
men and control temperatures in accordance with TGA manu- the final program temperature determi
...
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