Designation: D6375 − 09

Standard Test Method for

Evaporation Loss of Lubricating Oils by Thermogravimetric
Analyzer (TGA) Noack Method1
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—the oil provided by Noack equip-
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
procedure requires much smaller specimens, and is faster when 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. quickly heated to between 247 and 249°C under a stream of air,
1.4 This standard does not purport to address all of the and then held isothermal for an appropriate time. Throughout
safety concerns, if any, associated with its use. It is the this process, the TGA monitors and records the mass loss
responsibility of the user of this standard to establish appro- experienced by the specimen due to evaporation. The Noack
priate safety and health practices and determine the applica- evaporation loss is subsequently determined from the specimen
bility of regulatory limitations prior to use. weight percent loss versus time curve (TG curve) as the mass
percent lost by the specimen at the Noack reference time
2. Referenced Documents determined under the same TGA conditions.
2.1 ASTM Standards:2
D5800 Test Method for Evaporation Loss of Lubricating 5. Significance and Use
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
E1582 Practice for Calibration of Temperature Scale for 5.3 Some lubricant specifications cite a maximum allowable
Thermogravimetry evaporative loss.

1
6. Apparatus
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 6.1 Thermogravimetric Analyzer , with the capability to
D02.06 on Analysis of Lubricants. meet all the conditions required for this test method, along with
Current edition approved March 1, 2009. Published March 2009. Originally
the software necessary to complete the required analyses.
approved in 1999. Last previous edition approved in 2005 as D6375–05. DOI:
10.1520/D6375-09.
2
6.2 Aluminum Specimen Pan—This shall be cylindrical, and
For referenced ASTM standards, visit the ASTM website, [Link], or
have a minimum inside diameter/height ratio of 0.45 and a
contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on volume of 50 6 3 µL. If the pans provided by the particular
the ASTM website. TGA manufacturer do not meet these criteria, alternative pans

*A Summary of Changes section appears at the end of this standard

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 D6375 − 09

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. of 10 different pans and averaging the results. A caliper shall be
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- 9.1.2 Calculate the specimen mass using following equa-
ment. tion:
M s 5 350 ~ ID! 3 (1)
7. Reagents and Materials
Ms = Specimen mass, mg (round to closest whole mg.)
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
and describes their use in the operating manual for the 9.2 Air Flowrate— Set air flowrate to that recommended by
instrument. the TGA manufacturer or higher if during the initial tests with
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
of the internal parts of the TGA. 9.3 Temperature Program (see Note 2):
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
evaporative loss, the value of which is provided by the the method in the TGA.
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
an extended period of time, has had significant repairs made to it, or has
9.3.2 Program the TGA to heat the specimen from 50°C to
been mishandled or its location changed. the final program temperature determined in 9.3.1 at heating
rate(s) that will simulate the specimen heating rate of the
8.1 Check the temperature correlation between the speci-
standard Noack methods (;100°C/min to 220°C and 10°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 30
and regenerate correlation.
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 the TGA to 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 TGA gas 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.
specimen pan in the TGA during this operation. It will melt and 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 From the data obtained in 9.3.5, generate a plot of time
tions. versus specimen temperature. Determine whether at any time

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 D6375 − 09

FIG. 2 TGA Noack Programs and Resulting Specimen Heating Rates

the specimen temperature was above 249°C. When this occurs, reference oil and how to use it to determine the Noack
proceed to 9.3.8. When it does not occur, proceed to 9.3.7. reference time is shown in Fig. 4 (Curve 1). The isothermal
9.3.7 Temperature not over 249°C: Determine the Noack hold of the TGA temperature program can now be modified to
reference time in accordance with 9.4.6. When the Noack the Noack reference time plus 2 min. This will expedite future
reference time is less than 7 min, return to 9.3.2 and the reduce determinations.
heating rate to extend the Noack reference time beyond 7 min. 9.4.7 Check that the specimen temperature at the Noack
Check the specimen temperature at the Noack reference time to reference time is between 247 and 249°C. When the tempera-
be sure it is between 248 and 249°C. When it is lower, ture is outside this range, burn out TGA in accordance with 8.2
determine how much lower than 248.5°C and increase the final and repeat 9.4.
program temperature by this amount. Go to 9.4. 9.4.8 Compare the measured Noack reference time to those
9.3.8 Temperature over 249°C: Modify the TGA tempera- measured in prior days. When the difference is more than 10 %,
ture program to eliminate the temperature overshoot. This is check operation of the TGA in accordance with Section 8.
generally accomplished by splitting the program into two When significant repairs or modifications, such as replacement
stages, by reducing the heating rate by the final program of the balance mechanisms, temperature sensor, and so forth,
temperature, or by a combination thereof. An example of how have been made to the TGA since the previous time the Noack
temperature overshoot was eliminated in a particular instru- reference time was measured, the test method shall be repeated
ment is shown in Fig. 3. Repeat 9.3.3-9.3.6 until an appropriate starting with Section 8.
temperature program has been obtained.
9.5 Determination of TGA Noack Volatility of Test Lubri-
9.4 Determination of Noack Reference Time: cant:
NOTE 4—Important: This determination shall be completed each day 9.5.1 Using a new specimen pan, repeat 9.4.1-9.4.5 using
prior to evaluating any test specimens. the test lubricant in place of the Noack reference oil.
9.4.1 Set air flowrate in accordance with 9.2. 9.5.2 Using the TG curve for the test lubricant and the
9.4.2 Enter final temperature program established in 9.3. Noack reference time from 9.4.6, determine the mass loss (in
9.4.3 Tare an empty specimen pan in accordance with the mass %) of the test lubricant at the Noack reference time. This
TGA operating manual. is the TGA Noack volatility for the test lubricant. Examples of
9.4.4 Add the required mass (as determined in 9.1) of the how to determine the TGA Noack volatility of test lubricants
Noack reference oil to the tared pan. Whether specimen is are shown in Fig. 4 (Curves 2 and 3). Check that the specimen
added volumetrically or gravimetrically, the actual mass shall temperature at the Noack reference time is between 247 and
be within 63 mg of the calculated specimen mass. Adjust 250°C. When it is not, reinitiate the test starting with Section
specimen mass to meet this requirement. 8.
9.4.5 Place the pan on the TGA pan holder, and run 9.5.3 The TGA shall be burned out (see 8.2) on a regular
specimen. basis. An estimate of how many tests can be done on a
9.4.6 From the thermogravimetric curve generated in 9.4.5, particular TGA before it needs to be burned out can be obtained
determine the time (if possible to the closest 0.01 min) required by performing consecutive tests with the Noack reference oil
for the Noack reference oil to reach its Noack evaporative loss. until the difference in the Noack reference time between any of
This time is the Noack reference time. Record this time, as it the determinations is greater than 10 %. The number of tests
will be used in 9.5 to determine the TGA Noack volatility of between burn outs may be increased by operating at a higher
the test lubricants. An example of a TG curve for the Noack air flowrate (see 9.2).

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 D6375 − 09

FIG. 3 TGA Noack Programs and Resulting Specimen Heating Rates Showing Modification of TGA Program to Eliminate Overshoot in
Specimen Temperature

FIG. 4 Determination of Noack Reference Time and Test Oils Evaporative Loss

10. Report 12. Precision and Bias3

10.1 Report the TGA Noack volatility of the test lubricant, 12.1 On the basis of an interlaboratory round robin consist-
as determined in 9.5.2, to the closest 0.01 mass percent. ing of nine laboratories testing eight oils with TGA instruments
from five different manufacturers, the following precision and
11. Quality Control (QC) bias were determined for this procedure.
11.1 Confirm the performance of the instrument or the test 12.2 Repeatability— Two determinations made on the same
procedure by analyzing a QC sample. sample within a short interval of time, by the same operator
11.1.1 If a suitable QC oil or basestock sample is not using the same TGA equipment, in the normal and correct
available, prepare QC sample from a stock of such material. operation of this test method, should differ by more than the
11.1.2 When QC/Quality Assurance (QA) protocols are following value only in one case in twenty.
already established in the testing facility, they may be used
Repeatability 5 0.31 ~ TGA Noack Volatility! 0.60 (2)
when they confirm the reliability of the test result.
11.1.3 When there is no QC/QA protocol established in the
testing facility, Appendix X1 can be used as the QC/QA 3
Supporting data have been filed at ASTM International Headquarters and may
system. be obtained by requesting Research Report RR:D02-1447.

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 D6375 − 09
12.3 Reproducibility— Two determinations made on the 13. Keywords
same sample by different operators or using different TGA 13.1 evaporation loss of lubricants; Noack evaporative loss
equipment, in the normal and correct operation of this test by TGA; Noack volatility by TGA; TGA Noack volatility;
method, should differ by more than the following value only in
TGA volatility; thermogravimetry; volatility of lubricants
one case in twenty.
Reproducibility 5 0.39 ~ TGA Noack Volatility! 0.60 (3)
12.4 Bias—Within the repeatability of this test method, no
significant bias was found between the Noack volatility deter-
mined by this test method and those determined using Test
Method D5800.

APPENDIX

(Nonmandatory Information)

X1. QUALITY CONTROL (QC)

X1.1 Confirm the performance of the instrument or the test criticality of the quality being measured, the demonstrated
procedure by analyzing a quality control sample. stability of the testing process, and customer requirements.
Generally, a QC sample is analyzed each testing day with
X1.2 Prior to monitoring the measurement process, the user routine samples. The QC frequency should be increased if a
of this test method needs to determine the average value and large number of samples are routinely analyzed. However,
control limits of the QC sample. See Practice D6299 and when it is demonstrated that the testing is under statistical
MNL 7.4 control, the QC frequency may be reduced. The QC sample
X1.3 Record the QC results, and analyze by control charts precision should be checked against the ASTM test method
or other statistically equivalent techniques to ascertain the precision to ensure data quality.
statistical control status of the total testing process. See X1.5 It is recommended that, if possible, the type of QC
Practice D6299, Guide D6792, and MNL 7.4 sample that is regularly tested be representative of the material
X1.4 In the absence of explicit requirements given in the routinely analyzed. An ample supply of QC material should be
test method, the frequency of QC testing is dependent on the available for the intended period of use, and it must be
homogenous and stables under the anticipated storage condi-
tions. See Practice D6299, Guide D6792, or MNL 7,4 or a
4
MNL7, Manual on Presentation of Data Control Chart Analysis, 6th ed., ASTM combination thereof, for further guidance on QC and control
International, W. Conshohocken, PA. charting techniques.

SUMMARY OF CHANGES

Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D6375–05) that may impact the use of this standard.

(1) Deleted Other Documents from Section 2, including ac-

companying footnotes.

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 D6375 − 09
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