ASTM D6375-09(2014)
(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
SIGNIFICANCE AND USE
5.1 This test method is a safe and fast alternative for determination of the Noack evaporation loss of a lubricant.
5.2 The evaporation loss of a lubricant is important in the hot zones of equipment where evaporation of part of the lubricant may increase lubricant consumption.
5.3 Some lubricant specifications cite a maximum allowable evaporative loss.
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 mass %. This procedure requires much smaller specimens, and is faster when multiple samples are sequentially analyzed, and safer than the standard Noack method using Wood's metal.
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 standard. No other units of measurement are included in this 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.
General Information
Relations
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D6375 − 09 (Reapproved 2014)
Standard Test Method for
Evaporation Loss of Lubricating Oils by Thermogravimetric
Analyzer (TGA) Noack Method
This standard is issued under the fixed designation D6375; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method covers the procedure for determining 3.1 Definitions of Terms Specific to This Standard:
the Noack evaporation loss of lubricating oils using a thermo- 3.1.1 Noack reference oil—theoilprovidedbyNoackequip-
gravimetric analyzer test (TGA). The test method is applicable ment manufacturers to check proper operation of the Noack
to base stocks and fully formulated lubricant oils having a evaporation tester.
Noack evaporative loss ranging from 0 to 30 mass %. This
3.1.2 Noack reference time—the time (in minutes) required
procedurerequiresmuchsmallerspecimens,andisfasterwhen
for the Noack reference oil to reach its known Noack evapo-
multiple samples are sequentially analyzed, and safer than the
rative loss under the conditions used in this test method.
standard Noack method using Wood’s metal.
3.1.3 TGA Noack volatility—the evaporative loss (in mass
1.2 The evaporative loss determined by this test method is
percent) of a lubricant as determined in this test method.
the same as that determined using the standard Noack test
methods.
4. Summary of Test Method
1.3 The values stated in SI units are to be regarded as
4.1 A lubricant specimen is placed in an appropriate TGA
standard. No other units of measurement are included in this
specimen pan. The pan is placed on the TGA pan holder and
standard.
quicklyheatedtobetween247and249°Cunderastreamofair,
and then held isothermal for an appropriate time. Throughout
1.4 This standard does not purport to address all of the
this process, the TGA monitors and records the mass loss
safety concerns, if any, associated with its use. It is the
experienced by the specimen due to evaporation. The Noack
responsibility of the user of this standard to establish appro-
evaporationlossissubsequentlydeterminedfromthespecimen
priate safety and health practices and determine the applica-
weight percent loss versus time curve (TG curve) as the mass
bility of regulatory limitations prior to use.
percent lost by the specimen at the Noack reference time
2. Referenced Documents
determined under the same TGA conditions.
2.1 ASTM Standards:
5. Significance and Use
D5800 Test Method for Evaporation Loss of Lubricating
Oils by the Noack Method
5.1 This test method is a safe and fast alternative for
D6299 Practice for Applying Statistical Quality Assurance
determination of the Noack evaporation loss of a lubricant.
and Control Charting Techniques to Evaluate Analytical
5.2 The evaporation loss of a lubricant is important in the
Measurement System Performance
hot zones of equipment where evaporation of part of the
D6792 Practice for Quality System in Petroleum Products
lubricant may increase lubricant consumption.
and Lubricants Testing Laboratories
5.3 Somelubricantspecificationsciteamaximumallowable
E1582 Practice for Calibration of Temperature Scale for
evaporative loss.
Thermogravimetry
6. Apparatus
This test method is under the jurisdiction of ASTM Committee D02 on
6.1 Thermogravimetric Analyzer , with the capability to
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
meetalltheconditionsrequiredforthistestmethod,alongwith
CurrenteditionapprovedMay1,2014.PublishedJuly2014.Originallyapproved
the software necessary to complete the required analyses.
in 1999. Last previous edition approved in 2009 as D6375 – 09. DOI: 10.1520/
D6375-09R14.
6.2 Aluminum Specimen Pan—This shall be cylindrical, and
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
have a minimum inside diameter/height ratio of 0.45 and a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
volume of 50 6 3 µL. If the pans provided by the particular
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. TGA manufacturer do not meet these criteria, alternative pans
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6375 − 09 (2014)
FIG. 1 Examples Showing Adaptation of Alternative Sample 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
used to make this measurement.
6.4 Flowmeter, with a flow control valve capable of setting
9.1.2 Calculate the specimen mass using following equa-
and measuring the air throughput required by the TGA instru-
tion:
ment.
M 5 350 ~ID! (1)
s
7. Reagents and Materials
M = Specimen mass, mg (round to closest whole mg.)
s
7.1 TGA Temperature Calibration Standards—These mate-
ID = Nominal inside diameter of specimen pan, cm (see
rials will depend on the particular TGA apparatus and its
9.1.1).
capabilities. The TGA manufacturer typically provides them
9.2 Air Flowrate— Set air flowrate to that recommended by
and describes their use in the operating manual for the
the TGA manufacturer or higher if during the initial tests with
instrument.
the Noack reference oil there appears to be condensation on
7.2 Compressed air at a pressure suitable for operation of
any part of the TGA balance mechanism or furnace lining.
the TGA instrument. Reagent grade air is not necessary but
Repeat 8.1 with the new flow rate.
may be used if there are concerns over possible contamination
9.3 Temperature Program (see Note 2):
of the internal parts of the TGA.
7.3 Noack Reference Oil—Oil having a known Noack NOTE 2—This section only needs to be done during the initial set up of
the method in the TGA.
evaporative loss, the value of which is provided by the
manufacturer. 9.3.1 Using the correlation from 8.1, determine the final
program temperature required to obtain a final specimen
8. TGA Preparation and Calibration (see Note 1)
temperature of 249°C.
NOTE 1—This section only needs to be done if TGA has been idle for
9.3.2 Program the TGA to heat the specimen from 50°C to
an extended period of time, has had significant repairs made to it, or has
the final program temperature determined in 9.3.1 at heating
been mishandled or its location changed.
rate(s) that will simulate the specimen heating rate of the
8.1 Check the temperature correlation between the speci-
standardNoackmethods(;100°C/minto220°Cand10°C/min
men and control temperatures in accordance with TGA manu-
from 220°C to 249°C). Some guidance on how to achieve
facturer’s recommendations or Practice E1582. Use calibration
acceptable heating rates can be obtained from the examples
standards that will bracket 250°C.When necessary, recalibrate,
shown in Fig. 2. Maintain the final program temperature for
and regenerate correlation.
30 min (see Note 3).
8.2 When necessary, burn out the TGA to remove any
NOTE 3—The 30 min isothermal hold may be adjusted after the Noack
condensed liquids or deposits, which may have formed on its
reference oil has been tested and the Noack reference time for the
inside surfaces. Generally, burn out is accomplished by raising
instrument has been established (see 9.4).The isothermal hold can then be
the temperature of theTGAto a minimum of 800°C with an air
set to be 2 min longer than the measured Noack reference time.
purge from 200 to 500 mL/min, and by maintaining it at this
9.3.3 Tare an empty specimen pan in accordance with the
high temperature until no smoke is detected from the TGAgas
TGA operating manual.
exhaust tube. Normally 15 to 20 min at these conditions are
9.3.4 Add the required mass (6 3 mg) (as determined in
enough to remove most deposits. (Warning—Do not place a
9.1) of the Noack reference oil to the tared pan.
specimenpanintheTGAduringthisoperation.Itwillmeltand
9.3.5 Place the pan on the TGA pan holder, and run
may damage the balance or furnace mechanisms.)
specimen through the temperature program, as described in
8.3 Check operation of TGA balance and adjust when 9.3.2.
necessary. Follow manufacturer’s procedure and recommenda- 9.3.6 Fromthedataobtainedin9.3.5,generateaplotoftime
tions. versus specimen temperature. Determine whether at any time
D6375 − 09 (2014)
FIG. 2 TGA Noack Programs and Resulting Specimen Heating Rates
the specimen temperature was above 249°C.When this occurs, the test lubricants. An example of a TG curve for the Noack
proceed to 9.3.8. When it does not occur, proceed to 9.3.7.
reference oil and how to use it to determine the Noack
9.3.7
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6375 − 09 D6375 − 09 (Reapproved 2014)
Standard Test Method for
Evaporation Loss of Lubricating Oils by Thermogravimetric
Analyzer (TGA) Noack Method
This standard is issued under the fixed designation D6375; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope*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 mass %. This procedure requires much smaller specimens, and is faster when multiple
samples are sequentially analyzed, and safer than the standard Noack method using Wood’s metal.
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 standard. No other units of measurement are included in this 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.
2. Referenced Documents
2.1 ASTM Standards:
D5800 Test Method for Evaporation Loss of Lubricating Oils by the Noack Method
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
E1582 Practice for Calibration of Temperature Scale for Thermogravimetry
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 Noack reference oil—the oil provided by Noack equipment manufacturers to check proper operation of the Noack
evaporation tester.
3.1.2 Noack reference time—the time (in minutes) required for the Noack reference oil to reach its known Noack evaporative
loss under the conditions used in this test method.
3.1.3 TGA Noack volatility—the evaporative loss (in mass percent) of a lubricant as determined in this test method.
4. Summary of Test Method
4.1 A lubricant specimen is placed in an appropriate TGA specimen pan. The pan is placed on the TGA pan holder and quickly
heated to between 247 and 249°C under a stream of air, and then held isothermal for an appropriate time. Throughout this 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 specimen weight percent loss versus time curve (TG curve) as the mass percent lost by the
specimen at the Noack reference time determined under the same TGA conditions.
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 Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.06 on Analysis of Lubricants.
Current edition approved March 1, 2009May 1, 2014. Published March 2009July 2014. Originally approved in 1999. Last previous edition approved in 20052009 as
D6375D6375 – 09.–05. DOI: 10.1520/D6375-09.10.1520/D6375-09R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6375 − 09 (2014)
FIG. 1 Examples Showing Adaptation of Alternative Sample Pans
5.2 The evaporation loss of a lubricant is important in the hot zones of equipment where evaporation of part of the lubricant
may increase lubricant consumption.
5.3 Some lubricant specifications cite a maximum allowable evaporative loss.
6. Apparatus
6.1 Thermogravimetric Analyzer , with the capability to meet all the conditions required for this test method, along with the
software necessary to complete the required analyses.
6.2 Aluminum Specimen Pan—This shall be cylindrical, and have a minimum inside diameter/height ratio of 0.45 and a volume
of 50 6 3 μL. If the pans provided by the particular TGA manufacturer do not meet these criteria, alternative pans may be used
and adapted to fit the pan holder of the TGA. Examples of some of the adaptations used during the evaluation of this test method
are shown in Fig. 1.
6.3 Pressure Regulator, capable of maintaining air delivery pressure at the level required by the TGA instrument.
6.4 Flowmeter, with a flow control valve capable of setting and measuring the air throughput required by the TGA instrument.
7. Reagents and Materials
7.1 TGA Temperature Calibration Standards—These materials will depend on the particular TGA apparatus and its capabilities.
The TGA manufacturer typically provides them and describes their use in the operating manual for the instrument.
7.2 Compressed air at a pressure suitable for operation of the TGA instrument. Reagent grade air is not necessary but may be
used if there are concerns over possible contamination of the internal parts of the TGA.
7.3 Noack Reference Oil—Oil having a known Noack evaporative loss, the value of which is provided by the manufacturer.
8. TGA Preparation and Calibration (see Note 1)
NOTE 1—This section only needs to be done if TGA has been idle for an extended period of time, has had significant repairs made to it, or has been
mishandled or its location changed.
8.1 Check the temperature correlation between the specimen and control temperatures in accordance with TGA manufacturer’s
recommendations or Practice E1582. Use calibration standards that will bracket 250°C. When necessary, recalibrate, and
regenerate correlation.
8.2 When necessary, burn out the TGA to remove any condensed liquids or deposits, which may have formed on its inside
surfaces. Generally, burn out is accomplished by raising the temperature of the TGA to a minimum of 800°C with an air purge
from 200 to 500 mL/min, and by maintaining it at this high temperature until no smoke is detected from the TGA gas exhaust tube.
Normally 15 to 20 min at these conditions are enough to remove most deposits. (Warning—Do not place a specimen pan in the
TGA during this operation. It will melt and may damage the balance or furnace mechanisms.)
8.3 Check operation of TGA balance and adjust when necessary. Follow manufacturer’s procedure and recommendations.
9. Procedure
9.1 Determination of Specimen Mass :
9.1.1 Determine the nominal internal diameter (in centimetres) of the specimen pans by measuring the internal diameter of 10
different pans and averaging the results. A caliper shall be used to make this measurement.
9.1.2 Calculate the specimen mass using following equation:
M 5 350 ID (1)
~ !
s
M = Specimen mass, mg (round to closest whole mg.)
s
ID = Nominal inside diameter of specimen pan, cm (see 9.1.1).
D6375 − 09 (2014)
FIG. 2 TGA Noack Programs and Resulting Specimen Heating Rates
9.2 Air Flowrate— Set air flowrate to that recommended by the TGA manufacturer or higher if during the initial tests with the
Noack reference oil there appears to be condensation on any part of the TGA balance mechanism or furnace lining. Repeat 8.1 with
the new flow rate.
9.3 Temperature Program (see Note 2):
NOTE 2—This section only needs to be done during the initial set up of the method in the TGA.
9.3.1 Using the correlation from 8.1, determine the final program temperature required to obtain a final specimen temperature
of 249°C.
9.3.2 Program the TGA to heat the specimen from 50°C to the final program temperature determined in 9.3.1 at heating rate(s)
that will simulate the specimen heating rate of the standard Noack methods (;100°C/min to 220°C and 10°C/min from 220°C to
249°C). Some guidance on how to achieve acceptable heating rates can be obtained from the examples shown in Fig. 2. Maintain
the final program temperature for 30 min 30 min (see Note 3).
NOTE 3—The 30 min isothermal hold may be adjusted after the Noack reference oil has been tested and the Noack reference time for the instrument
has been established (see 9.4). The isothermal hold can then be set to be 2 min longer than the measured Noack reference time.
9.3.3 Tare an empty specimen pan in accordance with the TGA operating manual.
9.3.4 Add the required mass (6 3 mg) (as determined in 9.1) of the Noack reference oil to the tared pan.
9.3.5 Place the pan on the TGA pan holder, and run specimen through the temperature program, as described in 9.3.2.
9.3.6 From the data obtained in 9.3.5, generate a plot of time versus specimen temperature. Determine whether at any time the
specimen temperature was above 249°C. When this occurs, proceed to 9.3.8. When it does not occur, proceed to 9.3.7.
9.3.7 Temperature not over 249°C: Determine the Noack reference time in a
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.