Evaporation Loss of Lubricating Oils by The Noack Method: Standard Test Method For

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5800 − 21
Standard Test Method for

Evaporation Loss of Lubricating Oils by the Noack Method1
This standard is issued under the fixed designation D5800; 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* D4057 Practice for Manual Sampling of Petroleum and

1.1 This test method covers four procedures for determining Petroleum Products
the evaporation loss of lubricating oils (particularly engine D4177 Practice for Automatic Sampling of Petroleum and
oils). The evaporation measured is reported as percent total Petroleum Products
loss. The test method relates to one set of operating conditions D6299 Practice for Applying Statistical Quality Assurance
but may be readily adapted to other conditions as required. and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
1.2 Procedure B and Procedure D that are in the main D6300 Practice for Determination of Precision and Bias
section of the test method provide equivalent results. Proce- Data for Use in Test Methods for Petroleum Products,
dures A and C, which are in Annex A1 and Annex A2, have Liquid Fuels, and Lubricants
equivalent results. It has been determined that Procedures A
and C show a slight bias when compared to Procedures B and 2.2 DIN Standards:3
D. Procedures B and D give slightly higher results versus DIN 1725 Specification for Aluminum Alloys
Procedures A and C on formulated engine oils, while Proce- DIN 12785 Specifications for Glass Thermometers
dures B and D give lower results versus Procedures A and C on
basestocks. Thus, a correction factor is utilized to convert 3. Terminology
between the two sets of Procedures based on the fluid type. 3.1 Definitions of Terms Specific to This Standard:
1.3 The values stated in SI units are to be regarded as 3.1.1 evaporation loss, n—of a lubricating oil by the Noack
standard. No other units of measurement are included in this method, that mass of volatile oil vapors lost when the oil is
standard. heated in a test crucible through which a constant flow of air is
drawn.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.1.2 volatility, n—the tendency of a liquid to form a vapor.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 4. Summary of Test Method
mine the applicability of regulatory limitations prior to use. 4.1 A measured quantity of sample is placed in an evapo-
1.5 This international standard was developed in accor- ration crucible or reaction flask that is then heated to 250 °C
dance with internationally recognized principles on standard- with a constant flow of air drawn through it for 60 min. The
ization established in the Decision on Principles for the loss in mass of the oil is determined.
Development of International Standards, Guides and Recom- 4.2 Interlaboratory tests have shown that Procedure A,
mendations issued by the World Trade Organization Technical Procedure B, Procedure C, and Procedure D yield statistically
Barriers to Trade (TBT) Committee. equivalent precision, with a correlation coefficient of R2 =
0.996 (see research report).
2. Referenced Documents
2.1 ASTM Standards:2 5. Significance and Use
5.1 The evaporation loss is of particular importance in
1
This test method is under the jurisdiction of ASTM Committee D02 on
engine lubrication. Where high temperatures occur, portions of
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of an oil can evaporate.
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
Current edition approved Oct. 1, 2021. Published October 2021. Originally
5.2 Evaporation may contribute to oil consumption in an
approved in 1995. Last previous edition approved in 2020 as D5800 – 20. DOI: engine and can lead to a change in the properties of an oil.
10.1520/D5800-21.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from Deutsches Institut für Normung e.V.(DIN), Am DIN-Platz,
the ASTM website. Burggrafenstrasse 6, 10787 Berlin, Germany, http://www.din.de.
*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
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D5800 − 21
5.3 Many engine manufacturers specify a maximum allow- recorded in the specimen when heated with the Woods metal
able evaporation loss. heater block. In the center of the heating block, there is a
5.4 Some engine manufacturers, when specifying a maxi- circular recess to insert the evaporative crucible. The jacket
mum allowable evaporation loss, quote this test method along heater is configured to ensure a direct contact with the crucible.
with the specifications. A mechanism is provided to open the jaws for crucible
insertion. Two catches on the block prevent the crucible from
5.5 The apparatuses used in Procedure C (see Annex A2) rising, and the base heater is spring loaded to ensure a direct
and Procedure D, also permit collection of the volatile oil contact with the crucible.
vapors for determination of their physical and chemical prop- 6.2.2 Evaporative Crucible, with screw cover (see Fig. 3).
erties. Elemental analysis of the collected volatiles may be The crucible is made of stainless steel (see Fig. 4). Above the
helpful in identifying components such as phosphorous, which support ring is the thread for the cover. The nickel-plated brass
has been linked to premature degradation of the emission cover (see Fig. 5) is hermetically sealed to the crucible by an
system catalyst. internal conical sealing surface. Three nozzles of hardened
Procedure B—Non-Woods Metal Apparatus steel (see Fig. 6) permit the air stream to pass through the
cover. The extraction tube (see Figs. 7 and 8), which slopes
6. Apparatus downward, leads from a threaded and sealed connection in the
6.1 The following procedure, Procedure B, describes an center of the cover.
automated test method that uses the same principle, and the 6.2.3 Temperature Probe—The specimen temperature mea-
same crucible as Procedure A. Only the heat transfer medium suring device shall have an accuracy of 0.5 °C, or better, and a
to the sample and lid are different. It does not use Woods alloy, resolution of 0.1 °C, or better. The probe is provided with a
and the sample temperature is directly monitored. calibration certificate of 250.0 °C with a precision of 60.1 °C.
Its diameter is 4 mm, and its position is as indicated in Fig. 4.
6.2 Noack Evaporative Testers4, (see Fig. 1 and Fig. 2 for It should be calibrated with appropriate procedure at appropri-
both models), comprising the following: ate frequency (minimum once a year).
6.2.1 Heating Block Unit, electrically heated by base and
jacket heaters, having a total power consumption sufficient to 6.3 Balance, capable of weighing at least 500 g to the
ensure a specimen temperature profile similar to the one nearest 0.01 g.
6.4 Crucible Clamp and Spanner.
4
6.5 Reamer, 2 mm diameter.
The sole source of supply of the apparatus known to the committee at this time
for the Model A/B (NCK2/NCK2 5G) is ISL (PAC LP), B.P. 70285 14653 Carpiquet 6.6 Ball Bearing, 3 mm to 5 mm diameter.
Cedex, Verson, France. If you are aware of alternative suppliers, please provide this
information to ASTM International Headquarters. Your comments will receive 6.7 Glassware Assembly, strictly identical to the description
careful consideration at a meeting of the responsible technical committee,1 which in A1.1.6 – A1.1.12 and A1.1.15 of Procedure A.
you may attend.
FIG. 1 Model A

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FIG. 2 Model B
FIG. 3 Crucible with Temperature Probe
6.8 Vacuum Pump.

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FIG. 5 Crucible Cover (continued)
6.10 Printer, to print the graphs of the specimen temperature

FIG. 4 Noack Cup (Detail 1 of Fig. 3)
and the vacuum recorded during the test.
6.11 TMC calibration of the instrument is required for
results used in API licensing of formulated automotive engine
oils. The calibration procedure is defined in the Lubricant Test
Monitoring System (LTMS) document that is maintained by
the ASTM Test Monitoring Center (TMC)5 and is governed by
the D02.B0.07 Volatility Surveillance Panel. LTMS severity
adjustments shall be applied to results used in API licensing of
FIG. 5 Crucible Cover (Detail 2 of Fig. 3) automotive engine oils (12.2.1).
NOTE 1—It is the perception of the D02.B0.07 Volatility Surveillance
Panel that maintaining crucible cup and lid pairings is a measure of good
practice which minimizes variability. Under authority of the D02.B0.07
6.9 Central Processing Unit (CPU), capable of controlling Volatility Surveillance Panel, it has determined that for D5800 Procedure
the specimen temperature, the vacuum, the time, the heating, B tests to be considered operationally valid on TMC calibrated
and the printing. The specimen is heated to 245.2 °C 6 0.5 °C instruments, crucible cups and lids are to be initially paired by the testing
with the temperature profile recorded in the specimen when lab and then remain paired for the entire life-cycle of the crucible set.
tested with a Woods metal apparatus (1 h at 250 °C) with Moreover, labs may implement and retire paired crucible sets as needed
but once initially paired for calibration and candidate product testing,
automatic test duration compensation. The automatic test crucible cups and lids must remain paired for all subsequent test runs.
duration compensation is used because a test may be started Cups and lids shall be engraved or indelibly marked to maintain unique
with a heating block at room temperature or at hot temperature identification. Note that the use of multiple cup-lid pairings does not affect
when several tests are carried without cooling phase. The CPU the TMC calibration status of an instrument.
automatically adjusts the pressure differential of 20 mm 6
0.2 mm. These conditions can be checked with the printed 5
ASTM Test Monitoring Center, 6555 Penn Avenue, Pittsburgh, PA 15206-4489,
report. http://www.astmtmc.org.

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FIG. 5 Crucible Cover (continued)

FIG. 6 Specimen Temperature Probe Positioning
7. Reagents and Materials

7.1 Cleaning Solvent—A mixture of naphtha and toluene is NOTE 2—It has been reported during testing high Noack oils using some
recommended for cleaning the crucible. (Warning— models that the thermocouple probe can become exposed when evapora-
tion loss is high. While the instrument will alarm to indicate that the
Flammable, vapor harmful.) Overnight soaking may be neces- temperature fluctuation is greater than allowed in the test method, the
sary. heater will not shut off. If not noticed, the oil can continue to heat to close
7.2 Noack Reference Fluid—Oil such as NCO-126 having a to its flash point, and one laboratory has reported the sample to flash when
the probe was removed at the end of the test. Hence, it is suggested to
known evaporative loss for use with all D5800 method contact the instrument manufacturer to remedy possible malfunction.
procedures. The value of which is provided by the manufac-
turer. 8.2 (Warning—Though the test method calls for a draft-
free area, the exhaust fumes from the evaporating oil must be
7.3 Insulated Gloves. ventilated to an outside source. Precaution shall be taken to
7.4 Drying Paper. avoid any possibility of fire or explosion.) (See Note A1.3.)
8.3 An alternate means for preventing draft described in
8. Hazards
Appendix X3 was not used in the development of the test
8.1 Safety Hazards—It is assumed that anyone using this method precision statement.
test method will either be fully trained and familiar with all
normal laboratory practices, or will be under the direct super- 9. Preparation of Apparatus
vision of such a person. It is the responsibility of the operator 9.1 To avoid disturbing the thermal equilibrium, the appa-
to ensure that all local legislative and statutory requirements ratus shall be assembled in a draft-free area Plexi-glass draft
are met. shields are available from the manufacturer, for the model
shown in Fig. 2, if drafts in the room cause thermal distur-
6
The sole source of supply of the reference fluid known to the committee at this bances (see Appendix X3).
time is Tannas Co., 4800 James Savage Rd., Midland, MI 48642. If you are aware
9.2 Prepare the automated apparatus for operation in accor-
of alternative suppliers, please provide this information to ASTM International
Headquarters. Your comments will receive careful consideration at a meeting of the dance with the manufacturer’s instructions for calibrating,
responsible technical committee,1 which you may attend. checking, and operating the equipment.

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FIG. 7 Extraction Tube (Stainless Steel) with Its Seal (Details 3 and 4 of Fig. 3)
10.4 Run the ball bearing through the extraction tube to

ensure that it is clear of contaminants.
10.5 Calibrate the vacuum measuring device in accordance
with the manufacturer’s instructions.
10.6 Weigh the empty cup without its cover to the nearest
0.01 g.
10.7 Weigh into the tared crucible 65.0 g 6 0.1 g of
reference fluid to a precision of 0.01 g. This mass is called M1.
10.8 Screw on the cover using the clamp and the spanner.
During this phase, make sure that the specimen will never
splash on the inside part of the cover. If this occurs, even only
one time, the test shall be repeated from 10.3.
10.9 Connect the specimen temperature probe to the instru-
ment.
10.10 Press down on the locking lever located on the front
FIG. 8 Extraction Tube Nut (Stainless Steel) (Detail 5 of Fig. 3)
of the heating block. Place the crucible in the heating block.
Rotate the crucible, securing the flange under the screw heads.
Adjust the final position of the extraction tube so that it is
9.3 Clean the glass bottles, the glass tubing, and the Y-piece located in front of the arm of the glass Y-piece, and release the
to prevent a build-up of condensate. locking lever.
NOTE 3—Condensate should not be allowed to build up in the 2 L glass 10.11 Connect the extraction tube to the arm of the glass
bottles. These should be washed out with solvent and dried before a Y-piece, and secure the connection with the clamp. Be sure that
maximum 2 cm of condensate collects. the stainless extraction tube, the male connection, and the right
arm of the Y-piece are properly aligned.
10. Verification
10.12 Start the test by following manufacturer’s instruc-
10.1 It is recommended that a Noack reference oil check,
tions. When the audible alarm signals the last 3 minutes of the
such as NCO-12, be run each day of operation. Switch the
test, turn off the alarm. Stay in front of the equipment, and be
instrument on a minimum of 30 minutes before running the test
prepared to disconnect the extraction tube.
to allow temperature stabilization of measurement circuitry
10.13 After 60 min, the test is automatically stopped, and
10.2 Make sure that the glassware assembly and the vacuum
the end of the test alarm sounds. Remove the specimen
pump are cleaned and all the connections are sealed.
temperature probe. Disconnect the extraction tube within 15 s
10.3 Thoroughly clean and dry all parts of the test cup and maximum. Press down the locking lever. Remove the crucible.
its accessories before starting the test. Check that the crucible Stop the audible alarm.
and cover are free from lacquer. Stubborn lacquer should be
removed by soaking in the appropriate solvent (see manufac- 10.14 Stand the crucible in a cold DI or distilled water bath
turer’s manual). Pass the reamer through each of the three to a minimum depth of 30 mm.
nozzles in the cover to ensure that they are clear. (Warning— 10.15 Check the printed report to ensure that the specimen
Using a reamer with a diameter larger than 2 mm can enlarge temperature and vacuum plotted curves stayed within the
the nozzles. This can lead to a wrong losses result due to indicated limits. Occasionally the electronics will generate
increased air flow.) erroneous noise spikes in the graphs. These spikes are evident

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by a rapid temperature or pressure excursion followed by a checking of these conditions can be done with the printed
rapid return to baseline conditions. These spikes are not cause report. Calculate evaporation loss, using the following equa-
for invalidating a test. If however, there are gradual tempera- tion:
ture and/or pressure drifts or excessive noise spikes beyond @ ~ M 1 2 M 2 ! /M 1 # 3 100 (2)
specified limits, perform the necessary system maintenance
and/or calibrations. In addition, ensure the apparatus complies where:
with the manufacturer’s instruction and that the procedure has M1 = B – A,
been adhered to. After these checks, rerun the test from 10.6. M2 = C – A,
A = empty crucible weight,
10.16 After 30 min, remove the crucible from the water B = crucible plus specimen weight, and
bath, dry the outside, and carefully remove the lid. This phase C = crucible plus specimen after the test.
is very critical. Make sure that the sample is never in contact
with the inside part of the lid. 12.2 Procedure B and D provide equivalent results (see
RR:D02-1887).7 Some consistent differences in results deter-
NOTE 4—It is very important during the manipulation of the crucible, at mined using Procedures A/C and B/D have been observed
the start and the end of the test, to not splash the internal face of the cover depending on the type of sample tested. A test result obtained
with the specimen in the cup. When this occurs, it leads to higher losses
and the test must be rerun. using one of the procedures can be transformed to an estimated
result on the basis of the other procedure as follows:
10.17 Reweigh the crucible without the lid to the nearest 12.2.1 Formulated Engine Oils—The following relation-
0.01 g. ships are based on the round robin test results on formulated
10.18 Calculate the M2 mass by subtracting the empty cup engine oils with volatilities in the range of 10.5 % to 21.5 %
mass from the mass measured in 10.7. Noack:
10.19 Calculate to the nearest 0.1 % M/M the evaporation Value by Noack Procedure B⁄D 5 1.030
loss of the reference fluid, using the following equation: 3 Value by Noack Procedure A⁄C(3)
@ ~ M 1 2 M 2 ! /M 1 # 3 100 (1) Value by Noack Procedure A⁄C 5 0.970
where: 3 Value by Noack Procedure B⁄D(4)

The 95 % confidence limits for the regression coefficient in
M1 = specimen mass before the test, and Eq 3 are 1.021 to 1.033; those for the coefficient in Eq 4 are
M2 = specimen mass after the test at 245.2 °C. 0.968 to 0.980.
10.20 Compare the result obtained against the given value When results are utilized for API licensing of automotive
for the reference fluid. If the result is within limits, proceed to engine oils, a severity adjustment (SA) shall be applied to the
Section 11. final result of Eq 2. The severity adjustment is determined from
10.21 If the result is not within the limits, check that the the TMC calibration procedure, as stated in 6.11.
apparatus complies with the manufacturer’s instruction and 12.2.2 The following relationships are based on round robin
that the procedure has been adhered to. test results on basestocks with volatilities in the range of 4 %
to 25 % Noack:
10.22 Recheck the evaporation loss of the reference oil. To
do so, proceed as described in 10.2. Value by Noack Procedure B⁄D 5 0.962
3 Value by Noack Procedure A⁄C(5)
11. Procedure Value by Noack Procedure A⁄C 5 1.039
11.1 Weigh into a tared crucible 65 g 6 0.1 g representative 3 Value by Noack Procedure B⁄D(6)
of test specimen to a precision of 0.01 g. The 95 % confidence limits for the regression coefficient in
Eq 5 are 0.950 to 0.959; those for the coefficient in Eq 6 are
NOTE 5—Sample in accordance with Practice D4057 or Practice 1.043 to 1.053.
D4177. NOTE 6—The results of Noack residue should not be rounded up before
using the multiplication factors given in Eq 3-6.
11.2 Proceed as described in 10.3 – 10.17.
11.3 Calculate to the nearest 0.1 % M/M the evaporation 13. Report
loss of the specimen, using Eq 1.
13.1 Report the following information:
13.1.1 The nearest 0.1 % M/M as evaporation loss (Test
12. Calculation
Method D5800, Procedure B).
12.1 Evaporation loss is obtained from the difference in 13.1.2 If a severity adjustment is applicable to the result, the
weight before and after test. The specimen is heated in non-adjusted value, the severity adjustment, and the severity-
accordance with the temperature profile recorded in the speci- adjusted value are to be reported.
men when tested with a Woods metal apparatus (1 h at 250 °C)
with automatic test duration compensation. The automatic test
duration compensation is used because a test may be started 7
Supporting data have been filed at ASTM International Headquarters and may
with a heating block at room temperature or at hot temperature be obtained by requesting Research Report RR:D02-1887. Contact ASTM Customer
when several tests are carried without cooling phase. The Service at service@astm.org.

7
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D5800 − 21
13.2 Conversion of values from either D5800 A/C or D5800 14.1 To estimate the precision of Procedure B, the test
B/D to the other: results from the interlaboratory study were analyzed following
13.2.1 Only if the nature of the test specimen is known with Practice D6300.
certainty, in other words, it is known to be either a basestock or
a formulated engine oil, the evaporation loss calculated in 14.2 The interlaboratory study included ten oils, three base
12.2.1 on the basis of either Procedure A/C or Procedure B/D oils, and seven finished oils, tested in thirty laboratories.
may be converted to an equivalent result on the basis of the 14.3 The precision of this test method, as determined by the
other procedure. The appropriate equation from those above statistical examination of the interlaboratory study test results,
should be selected and applied according to the type of the is as follows:
sample tested (formulated engine oil or basestock). 14.3.1 Repeatability—The quantitative expression for the
13.3 Report the converted result from Procedure A/C to random error associated with the difference between two
B/D, or Procedure B/D to A/C to the nearest 0.1 m % as independent results obtained under repeatability conditions
evaporation loss of the test sample as converted from the that would be exceeded with an approximate probability of 5 %
original procedure to the calculated basis procedure. (one case in 20 in the long run) in the normal and correct
13.4 If the nature of the test specimen is not known as being operation of the test method:
either a basestock or a formulated engine oil, the results of the Repeatability 5 0.1331 · X 0.7443 (7)
test using Procedure B or D must be identified as being run
under Procedure B or D and the value of percent evaporation where:
so obtained will require additional information on the nature of X = average of the two determinations under consideration.
the test specimen for calculations to be made to generate the 14.3.2 Reproducibility—A quantitative expression for the
standard value produced by Procedure A or C.
random error associated with the difference between two
13.4.1 Converted results should be reported as D5800 A/C
independent results obtained under reproducibility conditions
(converted from the results obtained by D5800 B/D) or as
that would be exceeded with an approximate probability of 5 %
D5800 B/D (converted from the results obtained by D5800
(one case in 20 in the long run) in the normal and correct
A/C).
operation of the test method:
14. Precision and Bias8 Reproducibility 5 0.2411· X 0.7443 (8)
NOTE 7—Noack S2, Procedure D equipment has been shown to be
equivalent in two separate studies (see RR:D02-1887).7 where:
X = average of the two determinations under consideration.
8
Supporting data have been filed at ASTM International Headquarters and may 14.4 Bias—Since there is no accepted reference suitable for
be obtained by requesting Research Report RR:D02-1785. Contact ASTM Customer
Service at service@astm.org. As determined by the round robin, no significant determining the bias for this procedure, no statement on bias is
difference in results exists between Procedure B and Procedure C. being made.

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Procedure D—Automated Non-Woods Metal Noack S2 16.2 Hydrocarbon Solvent, such as hexane.
Volatility Test Apparatus 16.3 Medium Volatility Reference Oil.
15. Apparatus9 16.4 High Volatility Reference Oil.
15.1 Noack S2 (Trademark) Instrument—Fig. 9, including 17. Preparation and Setup of the Apparatus
parts as follows:
15.1.1 Reaction Vessel and Heater, capable of heating a 17.1 Locate the instrument on a laboratory bench if possible
sample quickly to test temperatures of 250 °C. (rather than a hood) to minimize atmospheric pressure fluctua-
15.1.2 Teflon Lid Assembly. tion. Vent the vacuum pump outlet provided on the back of the
15.1.3 Coalescing Filter. instrument with a metal or plastic tube leading to a suitable
15.1.4 Pump Filter. exhaust outlet.
15.1.5 Orifice Tube. 17.2 Insert the thermocouple connector into the thermo-
15.1.6 Magnetic Cross Stir Bar. couple receptacle on the back of the cabinet.
15.1.7 Thermocouple, PT100. 17.3 Be sure that the inside of the reactor vessel is clean and
15.1.8 Viton O-rings. that the other hardware and tubing are free of any oil residue.
15.1.9 Coalescing Filter Cartridges.
15.1.10 Pump Filter Cartridges. 17.4 If collection of the volatilized oil is desired, clean the
coalescing filter housing with a hydrocarbon solvent, dry, and
15.2 Balance, capable of weighing at least 500 g to the install new filter cartridge.
nearest 0.01 g.
17.5 Turn on the main power switch located on the front
15.3 Beaker, 600 mL. panel.
15.4 Cork spacer, capable of supporting reaction vessel
during weighing. 18. Calibration
18.1 The Noack S2 should be warmed up at the beginning
16. Reagents and Materials of the day. The unit should be turned on with the heat and
16.1 Cleaning Solvent, such as VarClean, capable of remov- vacuum pump on for 15 min to 30 min before the first test. If
ing varnish. the electronics have already been on for at least 15 min, it is
only necessary to wait for the instrument to control the heater
9
The sole source of supply of the apparatus known to the committee at this time temperature to 175 °C 6 5 °C before the first run.
is Tannas Co., 4800 James Savage Rd., Midland, MI 48642. If you are aware of
alternative suppliers, please provide this information to ASTM International
18.2 Calibrate the thermocouple at 250 °C against a certi-
Headquarters. Your comments will receive careful consideration at a meeting of the fied thermometer or other standard temperature measuring
responsible technical committee,1 which you may attend. device and, if necessary, adjust the calibration offset on the
FIG. 9 Noack S2 Test Equipment

9
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D5800 − 21
temperature controller according to the manufacturer’s instruc- 19.10 Perform a leak check of the reaction vessel assembly
tions. This shall be performed semi-annually. as per the manufacturer’s instructions.
18.3 Calibrate the vacuum pressure to 2.0 cm of water using 19.11 Remove the heat-resistant stopper, turn the vacuum
the manufacturer’s instructions. This shall be performed switch “ON,” place the reaction vessel assembly in the heater
weekly. assembly, and connect the reaction vessel lid tubing to the
system connector.
18.4 Set stir motor speed to/by manufacturer’s
recommendations/instructions and shall be performed semi- 19.12 Start the reference run using the controller.
annually. 19.13 When the test is complete, the system will shut down
18.5 In addition to the procedures described above, TMC the vacuum pump and the heater (even with the switches still
calibration of the instrument is required for results used in API “ON”). In addition, an audible buzzer will sound, test complete
licensing of automotive engine oils. The calibration procedure light will illuminate, and the test complete screen will be
is defined in the Lubricant Test Monitoring System (LTMS) displayed.
document that is maintained by the ASTM Test Monitoring 19.14 Remove the sample thermocouple. Be careful not to
Center (TMC) and is governed by the D02.B0.07 Volatility bend the sample thermocouple during removal.
Surveillance Panel. LTMS severity adjustments shall be ap-
plied to results used in API licensing of automotive engine oils 19.15 Disconnect the Teflon lid tubing quick connect.
(22.1.1). 19.16 Use heat-resistant gloves to remove the reaction
vessel assembly.
19. Reference Check
19.17 Reset the controller.
19.1 It is recommended that the Noack reference oil check,
19.18 Carefully place the reaction vessel assembly in the
NCO-12, be run each day of operation and the orifice adjusted
cooling cup of cold water. Avoid tilting or jostling the reaction
if necessary (see manufacturer’s manual). If applicable, see
vessel assembly during this process so residual oil does not get
18.5 for the TMC certification process as defined by the LTMS
transferred to the Teflon lid assembly. The water level should
document.
be lower than the flange on the reaction vessel assembly to
19.2 Allow the unit to warm up with the pump on while prevent any contamination to the sample.
preparing the sample. The heater can stay at 175 °C continu-
19.19 Remove the coalescing filter housing assembly. Drain
ously.
the collected volatiles. Replace the filter element as required. If
19.3 Clean the reaction vessel and stir bar with solvent needed, reassemble coalescing filter housing assembly and
(hydrocarbon solvents such as cyclohexane, heptane, and so replace in the unit.
forth) and dry it prior to the next test. 19.20 Check the pump filter housing assembly to be sure the
19.4 Clean the lid assembly with solvent and wipe dry prior pump filter it is not wet or yellowed. Never leave liquid in the
to the next test. Periodically, run a pipe cleaner through the pump filter housing assembly. Replace the filter as needed.
orifice tube to ensure no blockage or restrictions exist. 19.21 Carefully remove the sample thermocouple from the
19.5 Place a clean reaction vessel with the stir bar on a thermocouple holder and clean with a scrub pad.
scale. Record and compare the weight with the previous run. 19.22 The reaction vessel assembly should be cool after
The weight of the empty, clean reaction vessel and stir bar approximately 15 min.
should consistently be within 60.05 g. If the comparative
weight is within tolerance of the previous weight, tare the 19.23 Carefully open the reaction vessel assembly. Slowly
scale. If not, check the reaction vessel and/or stir bar for move the Teflon lid assembly up to avoid splashing liquid onto
cleanliness. Reweigh, compare, and tare the scale. the underside of the lid.
19.6 Place 65 g 6 0.02 g of reference oil in the reaction NOTE 9—Some condensed volatiles may cling to the Teflon lid
vessel. The stir bar magnet may affect some balances. assembly. This is not concerning and has been taken into account in the
method. However, care should be taken not to splash additional material.
NOTE 8—It is recommended to use the stopper (supplied with the 19.24 Place the stopper on the scale, weigh, and record the
instrument) to minimize any interference between the magnet and the
balance.
weight of the reaction vessel and contents.
19.7 Place the lid assembly in the reaction vessel and close 19.25 Determine the amount of oil volatilized and divide by
by tightening the lid retaining ring. the initial sample weight to determine the weight loss percent-
age (see Section A2.8).
19.7.1 If measuring the percent volatiles collected, follow
the manufacturer’s recommendations. 19.26 Compare the result to the given value of the reference
fluid. If results are within limits, proceed to the sample
19.8 Check the system temperature. To start the test, the
procedure. If the result is not within the limits of the reference
system temperature must be between 170 °C and 180 °C.
fluid, check that the procedure has been followed and that the
19.9 Place the reaction vessel assembly on top of the unit apparatus is set up properly with no leaks. Check the calibra-
and insert the sample thermocouple. tion of the temperature controller and pressure sensing device.

10
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NOTE 10—Procedures for calibration of the temperature controller and 22. Calculation
pressure controller can be found in the Operations Manual for the
Selby-Noack II Volatility test. 22.1 Percent volatility is determined by mass loss found by
subtracting the combined weight of the flask bottom and oil
19.27 If no errors in setup or procedure are identified, after testing from their combined weight before the test.
proceed to changing the size of the orifice tube. The size should
be changed in increments of 0.05 mm, with each change NOTE 11—The percent volatility is obtained by taking the mass loss of
corresponding to a directly related change of about 0.3 % the reaction flask and dividing that by the exact mass of the test oil sample
recorded earlier: that is, if weight of the oil sample is 65.1 g and weight
evaporation loss. A larger orifice tube increases the volatile of the oil lost is 10.2 g, then (10.2 g ⁄65.1 g) × 100 = 15.67 %.
value and a smaller orifice tube decreases the volatile value.
Rerun the reference fluid after making any changes. 22.1.1 When results are utilized for API licensing of auto-
motive engine oils, a severity adjustment (SA) shall be applied
19.28 If problems persist, contact the instrument manufac- to the final result of Eq 2. The severity adjustment is deter-
turer. mined from the TMC calibration procedure, as stated in 18.5.
19.29 Drain and rinse the reaction vessel, stir bar, and lid NOTE 12—When results are utilized for API licensing of automotive
assembly and O-ring, and wipe with a clean towel to ensure engine oils, a severity adjustment (SA) shall be applied to the final result
that both are clean and dry. of Eq 3. The severity adjustment is determined from the TMC calibration
procedure, as stated in 18.5.
19.30 Check the vacuum flow with the inclined manometer 22.2 The mass of volatiles collected is obtained by subtract-
assembly once per month or if the daily reference oil value ing the coalescing filter assembly weight before the test from
begins to drift. its weight at the end of the test.
19.31 Once the system has reached 175 °C 6 5 °C, it is now NOTE 13—The percent of volatiles collected is obtained by dividing the
ready for the next run. mass of volatiles collected by the mass loss: that is, if the weight of the
empty coalescing filter assembly is 163.2 g and the weight of the filter
20. Sample Procedure assembly after volatilization gained 9.8 g, and if the weight loss shown by
22.1 is 10.2 g, then (9.8 g ⁄10.2 g) × 100 = 96.08 % of the volatiles were
20.1 Perform the steps from Section A2.5 substituting a test collected.
sample for the reference fluid. Evaporation Loss %=$ @ ~ B 2 A ! 2 ~ C 2 A ! # ⁄ ~ B 2 A ! % 3 100
20.2 Calculate the percent evaporation loss of the test (9)
sample to the nearest 0.1 %. where:
20.3 Collect the volatilized oil (if desired for further analy- A = reaction vessel + stir bar weight,
sis) from the coalescing filter. B = A + sample weight, and
C = B after 1 h of heating.
21. Cleaning
23. Report
21.1 Clean all of the hardware, with the exception of the
reaction flask bottom, with a suitable hydrocarbon solvent (for 23.1 Report the evaporation loss to the nearest 0.1 %.
example, hexane, heptane, cyclo-hexane).
24. Precision7
21.2 If the coalescing filter is to be used for collecting NOTE 14—Procedures B and D were shown to be equivalent in
volatilized oil, it can be cleaned while disassembled. Unscrew RR:D02-1887 and therefore the same precision is reported as Procedure
the collection cup, remove the filter cartridge, and clean with a B.
suitable hydrocarbon solvent (for example, hexane, heptane, 24.1 Repeatability—The quantitative expression for the ran-
cyclohexane). Upon reassembly, the filter cartridge can be dom error associated with the difference between two indepen-
replaced with a new, clean cartridge. The filter can also be dent results obtained under repeatability conditions that would
removed from the bracket, if necessary, for cleaning. be exceeded with an approximate probability of 5 %, one case
in 20, in the normal and correct operation of the test method:
21.3 Place 10 mL of a varnish removing solvent into the
reaction flask bottom. Insert clean paper towel into the solvent Repeatability = 0.1331X 0.7443 (10)
and wipe inside of flask thoroughly, removing any varnish that 24.2 Reproducibility—A quantitative expression for the ran-
may be present on the wall. Rinse carefully with hot water and dom error associated with the difference between two indepen-
dry. dent results obtained under reproducibility conditions that
21.4 If other parts develop a varnish film, clean these with would be exceeded with an approximate probability of 5 %
the same procedure as indicated in A2.6.5 or put the parts into (one case in 20 in the long run) in the normal and correct
a half/half water or full-strength solution of varnish remover operation of the test method:
overnight. Reproducibility = 0.2411X 0.7443 (11)
21.5 With a towel dampened with varnish removing solvent,
clean the end of the thermocouple. Wipe with towel dampened 25. Quality Control for Procedures A, B, C, and D
with hot water and dry to remove any remaining cleaning 25.1 Procedures A, B, C, and D require confirmation of the
solvent or wipe with emery paper. performance of the apparatus by analyzing a quality control

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(QC) sample. Procedures A and C are equivalent and Proce- 25.4 The frequency of QC testing is dependent on the
dures B and D are equivalent. demonstrated stability of the testing process, customer
25.2 Prior to monitoring the measurement process, the user requirements, and the recommendations of the equipment
of the test method needs to determine the average value and manufacturer. The QC sample precision should be periodically
control limits of the QC sample. (See Practice D6299 and checked against the ASTM test method precision to ensure data
MNL 7.10) quality.
25.3 Record the QC results and analyze by control charts or 25.5 It is recommended that, if possible, the type of QC
other statistically equivalent techniques to ascertain the statis- sample that is regularly tested be representative of the samples
tical control status of the total testing process. (See Practice routinely analyzed. An ample supply of QC sample material
D6299 and MNL 7.10) Any out-of-control data should trigger should be available for the intended period of use and must be
investigation for root cause(s). The results of this investigation homogeneous and stable under the anticipated storage condi-
may, but not necessarily, result in instrument recalibration. tions.
26. Keywords
10
ASTM MNL7, Manual on Presentation of Data Control Chart Analysis, 6th
ed., Section 3, Control Chart for Individuals, ASTM International, W. 26.1 evaporation loss of lubricants; Noack volatility; vola-
Conshohocken, PA 19428. tility of lubricants
ANNEXES
(Mandatory Information)
A1. PROCEDURE A—WOODS METAL APPARATUS
A1.1 Apparatus The thermometer should be calibrated with appropriate proce-

A1.1.1 Noack Evaporative Tester, comprising the following: dure at appropriate frequency (generally every six months).
A1.1.1.1 Electrically Heated Block Unit, made from a A1.1.7 Contact-Type Control Thermometer (for manual).
malleable aluminum alloy (see DIN 1725, Sheet 1), insulated at
the jacket and base against loss of heat. (Warning—This block A1.1.8 Glass Y-piece, an internal diameter of 4 mm. The
is heated to 250 °C.) The block is heated electrically by a base upright arms, each 45 mm long, should form an angle such that
and jacket heater, having a total power consumption of 1 kW to the arm connected to the crucible extraction tube and the
1.2 kW. In this respect the difference between both individual Y-piece form a straight line. The vertical arm is 60 mm long
power consumption should not exceed 0.15 kW. In the center and beveled at 45°.
of the heating block, there is a circular recess to insert the A1.1.9 Glass Delivery Tubes, an internal diameter of 4 mm,
evaporating crucible, the space between block and crucible each arm length 100 mm, beveled at 45° at ends entering and
being filled with Woods alloy or a suitable equivalent. Two leaving the bottles.
catches on the block prevent the crucible from rising in the A1.1.9.1 Bent at an angle of approximately 80°.
liquid metal bath. Two additional circular recesses at equal A1.1.9.2 Bent at an angle of approximately 100°, length to
intervals from the center of the block are provided for the 20 mm of bottle base.
thermometers (see Fig. A1.1). A1.1.9.3 Bent at an angle of approximately 90°.
A1.1.1.2 Evaporating Crucible, with screw cover. The cru-
cible is made of stainless steel (see Fig. A1.2). Above the A1.1.10 Two Glass Bottles, approximately 2 L capacity,
support ring is the thread for the cover. The nickel-plated brass fitted with rubber bungs bored to receive inlet and outlet tubes
cover is hermetically sealed to the crucible by an internal (see Fig. A1.4).
conical sealing surface (see Fig. A1.3). Three nozzles of A1.1.11 Manometer, inclined form, water-filled, precision
hardened steel permit the air stream to pass through the cover. 0.2 mm H2O or suitable pressure sensor capable of measuring
The extraction tube, which slopes downward, leads from a 20 mm 6 0.2 mm of H2O (a 0 mm to 50 mm H2O pressure
threaded and sealed connection in the center of the cover. transducer has been found to be satisfactory).
A1.1.2 Balance, capable of weighing at least 200 g to the
NOTE A1.1—Some manometers use water as the reference fluid, others
nearest 0.01 g. may use a lower density fluid correlated to read in millimetres of water.
A1.1.3 Crucible Clamp and Spanner. Users should ensure that the manometer is filled with the correct density
reference fluid.
A1.1.4 Reamer, 2 mm diameter.
A1.1.12 Glass T-Piece, with bleed valve attached.
A1.1.5 Ball Bearing, 3.5 mm diameter.
A1.1.13 Vacuum Pump.
A1.1.6 Thermometer, M260 (see DIN 12785) or tempera-
ture sensing device capable of reading temperature to 0.1 °C. A1.1.14 Timer, with accuracy of 0.2 s.

12
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NOTE 1—All dimensions in millilitres.

FIG. A1.1 Heating Block

13
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NOTE 1—All dimensions in millilitres.

NOTE 1—All dimensions in millilitres. FIG. A1.3 Cover
FIG. A1.2 Crucible
A1.1.15 Silicone Rubber Tubing, cut to size, with an inter-

nal diameter of 4 mm. A1.2.2 Noack Reference Fluid NCO-126—Oil having a
A1.1.15.1 40 mm long; three pieces required, known evaporative loss for use with all D5800 method
A1.1.15.2 300 mm long, and procedures. The value of which is provided by the manufac-
A1.1.15.3 100 mm long. turer.
NOTE A1.2—The use of automated equipment is permissible as long as
it gives equivalent results specified in this test method. All hardware A1.2.3 Insulated Gloves.
dimensions, make-up of the block, crucible, heat capacity, and so forth,
and glassware must conform to the specifications given in this test
A1.2.4 Paint Brush, such as a tinnerps acid brush (15 mm to
method. 25 mm width).
A1.2 Reagents and Materials

A1.2.1 Cleaning Solvent—A mixture of naphtha and toluene
is recommended for the cleaning of the crucible. (Warning—
Flammable, vapor harmful.) Overnight soaking may be neces-
sary.

14
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apparatus shall be assembled in a draft-free area and comply
with Fig. A1.5 in dimensions and apparatus. (See A1.3.2.)
A1.4.2 Add sufficient Woods metal or equivalent material to
the recesses of the heating block so that, with the crucible and
thermometer in place, the remaining spaces will be filled with
the molten metal.
A1.4.3 Using the highest heating rate possible, raise the
temperature of the heating block until the Woods metal is
molten. Insert the thermometers with their bulbs touching the
bottom of the recesses, and ensure that the contact thermometer
is plugged in the back of the heating block. Adjust the power
supplied to the heating block so that the temperature can be
maintained at 250 °C 6 0.5 °C.
A1.4.4 Assemble the remaining apparatus, less the crucible,
as shown in Fig. A1.5.
A1.4.5 Place an empty crucible in the heating block, secur-
ing the flange under the screw heads against the buoyancy of
the Woods metal. The level of the molten metal should be such
that a trace of it can be seen at the flange of the crucible and the
top of the heating block.
A1.4.6 Check that the readings can be obtained on the
FIG. A1.4 Glassware manometer scale, or other measuring device, by connecting the
crucible to the assembled apparatus. A reading of 20.0 mm 6
A1.2.5 Woods Metal11 or Suitable Heat Transfer Material— 0.2 mm shall be obtained.
(Warning—Woods metal contains lead (25 %), bismuth A1.4.7 Disconnect and remove the crucible from the as-
(50 %), antimony (12.5 %), and cadmium (12.5 %); these have sembled apparatus.
been found to be health hazardous. Avoid contact with skin at
all times.) A1.4.8 Switch off the pump and the heating block and raise
the crucible and the thermometers from the molten Woods
A1.3 Hazards metal. Using the brush, return any Woods metal clinging to the
A1.3.1 Safety Hazards—It is assumed that anyone using this crucible to the heating block.
test method will either be fully trained and familiar with all A1.4.9 Clean the Y-piece and glass tubing to prevent a
normal laboratory practices, or will be under the direct super- build-up of condensate.
vision of such a person. It is the responsibility of the operator
to ensure that all local legislative and statutory requirements A1.5 Verification
are met. A1.5.1 Switch on the pump and the heating block and
A1.3.2 (Warning—Though the test method calls for a ensure that the apparatus is assembled, minus the crucible, as
draft-free area, the exhaust fumes from the evaporating oil shown in Fig. A1.5.
must be ventilated to an outside source. Precaution shall be A1.5.2 Check that the crucible and cover are free from
taken to avoid any possibility of fire or explosion.) lacquer.
NOTE A1.3—One way to achieve a draft-free environment and greater A1.5.2.1 After every test, clean the crucible and cover with
safety in operation for the instruments used in this test method is described solvent and allow to dry. Stubborn lacquer can be cleaned by
in Appendix X3. abrasion from a glass beader under pressure.
A1.3.3 An alternate means for preventing draft described in A1.5.3 Pass the reamer through each of the three nozzles in
Appendix X3 was not used in the development of the test the cover to ensure that they are clear. (Warning—Using a
method precision statement. reamer with a diameter larger than 2 mm can enlarge the
nozzles. This can lead to higher losses because of increased air
A1.4 Preparation of Apparatus
flow.)
A1.4.1 A standard assembly of the apparatus is shown in
A1.5.4 Run the ball bearing through the extraction tube to
Fig. A1.5. To avoid disturbing the thermal equilibrium, the
ensure that it is clear of dirt.
11
The sole source of supply of Woods metal known to the committee at this time A1.5.5 Weigh the empty crucible without its cover to the
is Sigma-Aldrich, Customer Support, P.O. Box 14508, St. Louis, MO 63178. If you nearest 0.01 g.
are aware of alternative suppliers, please provide this information to ASTM
International Headquarters. Your comments will receive careful consideration at a A1.5.6 Weigh into the crucible 65.0 g 6 0.1 g of the
meeting of the responsible technical committee,1 which you may attend. reference oil.

15
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FIG. A1.5 Test Apparatus
A1.5.7 Screw on the cover using the clamp and spanner. the temperature and pressure differential remain constant
A1.5.8 Ensure the temperature of the heating block is at throughout the period of the test.
250 °C 6 0.5 °C. Place the crucible in its recess in the heating A1.5.11 After 60 min 6 5 s, lift the crucible from the
block, securing the flange under the screw heads against the heating block, remove any adhering alloy, and place the
buoyancy of the Woods metal. Switch the control of the heating crucible in a warm water bath to a depth of at least 30 mm. The
block to compensate for the heat capacity of the crucible. time period from the end of the test to immersion of the
Immediately (in less than 5 s), connect the extraction tube of crucible shall not exceed 60 s.
the crucible to the arm of the glass Y-piece, making a butt joint. A1.5.12 After 30 min, remove the crucible from the water,
Simultaneously, start the pump and the stopwatch and adjust dry the outside, and carefully remove the lid.
the bleed valve to give a pressure differential of 20 mm 6
0.2 mm. A1.5.13 Reweigh the crucible without the lid to the nearest
0.01 g.
NOTE A1.4—When the crucible is in the test position, its flange should
be flush with the top of the heating block. Any protrusion of the crucible A1.5.14 Calculate to the nearest 0.1 % mass ⁄mass (M/M)
flange above the heating block may suggest a buildup of Woods metal slag the evaporation loss of the reference oil.
at the bottom of the heating block recess. The heating block and the
thermometer recesses should be cleaned and the Woods metal replaced on A1.5.15 Compare the result obtained against the given
a regular basis to avoid the accumulation of slag. Oxidized Woods metal value for the reference oil. If the result is within 6 % of the
will affect the heat transfer to the crucible and hence may have a value, repeat the procedure from A1.6.1, using the test sample.
deleterious effect on the results obtained.
A1.5.16 If the result is not within 6 % of the given value,
A1.5.9 Adjust the control on the heating block to maintain check that the apparatus complies with that shown in Fig. A1.5,
the block temperature approximately 5 °C below the test and that the procedure has been adhered to. Check the
temperature. Readjust the temperature control so that the test calibration of the thermometer and pressure sensing device.
temperature is reestablished within 3 min of the start of the test.
A1.5.17 Re-check the evaporation loss of the reference oil.
NOTE A1.5—Temperature and pressure will be controlled automatically
when automated equipment is used. NOTE A1.6—Condensate should not be allowed to build up in the 2 L
glass bottles. These should be washed out with solvent before a maximum
A1.5.10 At the start of the test, constant attention shall be 1 cm of condensate collects.
paid to maintaining the correct pressure. Once this becomes NOTE A1.7—The equipment should be referenced approximately every
steady, usually within 10 min to 15 min, check periodically that ten tests if the test is used frequently. If the testing is infrequent, the

16
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equipment should be referenced before the first sample is run. A1.9 Precision and Bias12
A1.6 Procedure A1.9.1 The interlaboratory round robin used manual, semi-
automated, and automated equipment. The precision values
A1.6.1 Weigh into a tared crucible 65 g 6 0.1 g represen- were calculated on the statistical examinations of interlabora-
tative of the test sample to a precision of 0.01 g. tory test results as follows.
A1.9.1.1 Repeatability—The quantitative expression for the
NOTE A1.8—Sample in accordance with Practice D4057 or Practice
D4177. random error associated with the difference between two
independent results obtained under repeatability conditions
A1.6.2 Proceed as described in A1.5.7 – A1.5.12. that would be exceeded with an approximate probability of 5 %
A1.6.3 Calculate to the nearest 0.1 % M ⁄M the evaporation (one case in 20 in the long run) in the normal and correct
loss of the sample. operation of the test method:
Repeatability 5 5.8 % 3 average M/M evaporation loss (A1.2)
A1.7 Calculation and Results
A1.9.1.2 Reproducibility—A quantitative expression for the
A1.7.1 Evaporation loss is obtained from the difference in random error associated with the difference between two
weight before and after 1 h at 250 °C. independent results obtained under reproducibility conditions
~B 2 A! 2 ~C 2 A! that would be exceeded with an approximate probability of 5 %
evaporation loss 5 3 100 (A1.1) (one case in 20 in the long run) in the normal and correct
B2A
where:
Reproducibility 5 18.3 % 3 average M/M evaporation loss
A = empty crucible weight,
(A1.3)
B = crucible plus sample weight, and
C = crucible plus sample after 1 h of heating. A1.9.2 The procedure in this test method has no bias
because the value of the volatility is defined only in terms of
A1.8 Report this test method.
A1.8.1 Report the following information: 12
Supporting data have been filed at ASTM International Headquarters and may
A1.8.1.1 The nearest 0.1 % M/M as evaporation loss (Test be obtained by requesting Research Report RR:D02-1462. Contact ASTM Customer
Method D5800). Service at service@astm.org.
A2. PROCEDURE C—SELBY-NOACK VOLATILITY TEST
A2.1 Apparatus9 A2.1.1.10 Measuring Rod, of known length.

A2.1.1 Selby-Noack Instrument, (see Fig. A2.1) including A2.1.1.11 Viton O-Rings.
glassware and other parts as follows: A2.1.1.12 Coalescing Filter Cartridges.
A2.1.1.1 Reaction Flask Bottom, capable of heating a A2.1.1.13 Pump Filter Cartridges.
sample quickly to test temperatures of 250 °C. A2.1.2 Balance, capable of weighing at least 300 g to the
A2.1.1.2 Reaction Flask Top. nearest 0.01 g.
A2.1.1.3 Coalescing Filter.
A2.1.1.4 Pump Filter. A2.1.3 Beaker, 600 mL.
A2.1.1.5 Orifice Tube. A2.1.4 Cork Ring, capable of supporting collection flask
A2.1.1.6 Orifice Cap, of a set of incremental sizes. during weighing.
A2.1.1.7 Thermocouple Sheath.
A2.1.1.8 Magnetic Stir Bar. A2.1.5 Digital Timer.
A2.1.1.9 Thermocouple. A2.1.6 Tapered Glass Adapter.

17
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FIG. A2.1 Selby-Noack Test Equipment
A2.2 Reagents and Materials A2.3.2.4 Turn the tapered plastic piece on the orifice tube
A2.2.1 Cleaning Solvent, such as VarCleen, capable of toward the top of threaded section and be sure the orifice cap
removing varnish from glassware. is removed.
A2.3.2.5 Temporarily assemble the top and bottom pieces of
A2.2.2 Hydrocarbon Solvent, such as hexane.
the reactor and put the orifice tube in position.
A2.2.3 Average Volatility Reference Oil. A2.3.2.6 Insert the measuring rod through the orifice tube.
A2.2.4 High Volatility Reference Oil. When the lower end of the rod is in contact with the reactor
A2.2.5 Pump Oil, suitable for vacuum pump installed in bottom, the lower surface of the collar should be above the
instrument. upper end of the orifice tube.
A2.3.2.7 Adjust the tapered plastic piece on the orifice
A2.3 Preparation of Apparatus down to achieve very light contact between the upper end of
A2.3.1 Locate the instrument on a laboratory bench if the orifice tube and the lower surface of the collar on the
possible (rather than a hood) to minimize atmospheric pressure measuring rod to establish the proper position.
fluctuation. Vent the vacuum pump outlet provided on the back
A2.3.3 Insert the two thermocouple connectors into the
of the instrument with a metal or plastic tube leading to a
thermocouple receptacles on the cabinet.
suitable exhaust outlet. Whether the instrument is placed on the
bench or in a hood, make sure the instrument’s built-in door A2.3.4 Insert the heater cable into the heater connection on
(which serves as both draft control and safety shield) is firmly the cabinet.
closed and latched for all calibrations and tests as illustrated in
Fig. A2.1. A2.3.5 Be sure that the inside of the reactor bottom is clean
(see A2.6.5) and that the other glassware, hardware, and tubing
A2.3.2 Set the height of the outlet of the orifice tube are free of any oil residue.
11.4 cm above the inside bottom of the reaction flask.
A2.3.2.1 Measure the length of the measuring rod and the A2.3.6 If collection of the volatilized oil is desired, clean
length of the orifice tube (without the cap) in centimetres. the coalescing filter housing with a hydrocarbon solvent, dry,
A2.3.2.2 Add the measured length of the orifice tube with- and install new filter cartridge.
out the orifice cap to 11.4 cm. A2.3.7 Turn on the main power switch located on the front
A2.3.2.3 Use the value obtained in A2.3.2.2 to set the length
panel.
of the measuring rod by affixing the collar at that height. This
will give the desired value from the lower tip of the measuring A2.3.8 Before operating the instrument close the shield
rod up to the bottom of the collar. door.

18
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A2.4 Calibration A2.4.15 Connect the hose from the pressure sensor to the
barbed connection on the reaction flask top next to the sidearm.
A2.4.1 Calibrate the thermocouple at 100 °C or higher
After connections are made, check that the reaction flask top is
against a certified thermometer or other standard temperature
horizontal with the reaction flask bottom and that the O-ring
measuring device and, if necessary, adjust the calibration offset
seal between them is in proper position.
on the temperature controller according to the manufacturer’s
instructions. A2.4.16 Slide the thermocouple into the thermocouple
sheath in such a manner that the plastic tubing seals the joint
A2.4.2 Preheat reaction flask bottom by placing the clean
between the thermocouple and the thermocouple sheath. This
flask (with magnetic stirrer inside) on the reaction flask
will ensure no leaks.
platform. Place the thermocouple inside the flask and be sure
that the tip is firmly touching the inside wall. Set the tempera- A2.4.17 Make certain that the thermocouple contacts the
ture controller for 100 °C and turn on the heater switch. When wall. This can be viewed by looking down through the top of
the temperature reaches 100 °C, start the timer for 5 min. the reaction flask top. It is important that the thermocouple
touches the inside wall of the reaction flask at least 0.5 in.
A2.4.3 After the 5 min has expired, turn off the heater
below the surface of the oil for proper results.
switch and wait for the flask to cool below 50 °C. After
cooling, check the dry weight of the reaction flask bottom A2.4.18 With the vacuum control Open/Close switch set to
against the weight of previous weighings. the middle or Flow position, turn on the Vacuum On/Off switch
on the upper console.
NOTE A2.1—The sequential weighings should be reasonably constant
(that is, within 60.02 g) although the weight will decrease in a regular A2.4.19 Press down the Gauge Factor/Flow/Set Pt. switch
way over days and months of use. Any sudden increase in weight or erratic and, using the Set Point dial, adjust the vacuum to 2.00 cm
fluctuation is an indication that the outside insulating coating of the
bottom reaction flask has been contaminated and the flask should be
(20 mm) of water on the meter readout. When at a reading of
repeatedly baked according to A2.4.2 until constant weight is reestab- 2.00, release the Gauge Factor/Flow/Set Pt. switch.
lished.
A2.4.20 Press one finger tightly over the hole in the orifice
A2.4.4 Weigh the flask with the stirring bar and record the cap and toggle the vacuum control Open/Close switch to the
value to the nearest 0.01 g. closed position. The vacuum reading should increase to a
stable value (this must be below 19.00 cm of water). Once
A2.4.5 Pour 65 g 6 0.02 g of reference oil into the reaction
stabilized and with finger still in place, turn the vacuum pump
flask. Record the mass of the oil to the nearest 0.01 g.
off and monitor the vacuum to observe how well it maintains
A2.4.6 Insert the appropriate orifice cap size into orifice the vacuum. Remove finger from the orifice cap and again
tube, making certain there is a good seal. Insert the orifice tube monitor the vacuum; it should quickly decrease to a zero
(with the orifice cap) into the center glass tapered joint on the reading.
reaction flask top and make certain it has seated properly.
A2.4.21 If there is a leak, recheck all of the glass fittings, the
A2.4.7 Insert the thermocouple sheath, without the orifice tube, and the thermocouple sheath for proper seating.
thermocouple, into the thermocouple connection on the reac- Repeat step A2.4.20. If there is no leak then continue to
tion flask top with the bend facing away from the glass A2.4.22.
sidearm.
NOTE A2.2—High-temperature vacuum grease may be used to seal
A2.4.8 Join the reaction flask top and bottom and insert the leaks, if necessary. Vacuum grease should not be used on components that
assembly into the flask clip provided. are weighed during the test procedure.
A2.4.9 Raise the stirrer platform to stabilize the reaction A2.4.22 With the vacuum switch already on and controlling
flask bottom. at 2.00 cm of water, turn on the stirrer. Visually verify the
stirring.
A2.4.10 If collection of volatiles is desired, weigh the clean
coalescing filter assembly including the filter cartridge and A2.4.23 Set the temperature controller to 250 °C and turn
record the results to the nearest 0.01 g. on the heater switch. An automatic timer will activate when the
heater switch is turned on. The timer will turn off the heater,
A2.4.11 Mount to bracket with the arrow pointing in the vacuum, and stirring motor after 1 h.
direction of air flow (toward the vacuum pump).
A2.4.24 Allow the unit to cool down to a temperature safe
A2.4.12 Connect the inlet coalescer tubing to the barbed for handling (approximately 20 min). Gloves may be used to
end of the tapered glass adapter (which will be later connected handle while hot.
to the reaction flask top sidearm).
A2.4.25 Weigh the volatilized oil (if desired).
A2.4.13 Connect the tubing to the input side of the coalesc- A2.4.25.1 Remove the tubing from the coalescing filter
ing filter and connect the tapered glass adapter to the reaction assembly and remove the assembly from the bracket.
flask top sidearm and secure with a glass joint clamp.
A2.4.25.2 Weigh the entire coalescing filter assembly and
A2.4.14 Connect the vacuum hose from the pump filter record the results to the nearest 0.01 g. Subtract previous dry
(above the coalescing filter) to the output connection on the assembly weight from A2.4.10 to obtain the weight of volatil-
coalescing filter. ized oil.

19
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A2.4.25.3 Save the volatilized oil, if desired, by draining NOTE A2.5—It is recommended that a reference fluid be tested to
out through the petcock in the bottom of the coalescing filter confirm calibration at the beginning of each series of sample tests and at
the beginning of every other day of continuous testing. If testing is not
housing. conducted on a daily basis, test the reference fluid at the beginning of each
A2.4.26 Remove the pressure sensor tube and the test day. If the percent evaporation loss of the reference fluid is not within
thermocouple, and then remove the reaction flask top. The limits, check the instrument for operating precision or recalibrate before
samples are tested, or both.
orifice tube and thermocouple sheath may be left in position
during cleaning and reassembly. (If any oil is clinging to the A2.6 Cleaning
sheath tip, touch it to the side wall of the reactor bottom to
return it to the reaction flask.) A2.6.1 Clean all of the glassware and hardware, with the
exception of the reaction flask bottom, with a suitable hydro-
A2.4.27 Weigh and record the reaction flask bottom plus carbon solvent (for example, hexane, heptane, cyclo-hexane).
remaining residual oil to the nearest 0.01 g and either discard
or save the residual oil for further analysis. A2.6.2 If the coalescing filter is to be used for collecting
volatilized oil, it can be cleaned while disassembled. Unscrew
A2.4.28 Clean all glassware and hardware as described in the collection cup, remove the filter cartridge, and clean with a
A2.6.1 – A2.6.7. suitable hydrocarbon solvent (for example, hexane, heptane,
A2.4.29 Calculate the percent volatility loss of the reference cyclo-hexane). Upon reassembly, the filter cartridge can be
fluid to the nearest 0.1 % (see Section A2.7). replaced with a new, clean cartridge. The filter can also be
A2.4.30 Compare the result to the given value of the removed from the bracket, if necessary, for cleaning.
reference fluid. If results are within limits, proceed to the A2.6.3 In order to prevent oil from coming into contact with
Sample Procedure. the outside of the reaction flask bottom, wrap the outside lip of
A2.4.31 If the result is not within the limits of the reference the reaction flask bottom with clean toweling and quickly pour
fluid, check that the procedure has been followed and that the out the contents into a beaker in order to catch the stir bar.
apparatus is set up properly with no leaks. Check the calibra- While still holding the flask upside down remove the towel,
tion of the temperature controller and pressure sensing device. wipe the lip dry, and then carefully rinse the inside of the flask
NOTE A2.3—Procedures for calibration of the temperature controller with a hydrocarbon solvent. When the unit is clean, wipe it dry
and pressure controller can be found in the Operations Manual for the with another towel.
Selby-Noack Volatility test.
NOTE A2.6—If the insulating covering of the reaction flask bottom
A2.4.32 If no errors in setup or procedure are identified, becomes contaminated, follow the directions in Note A2.1.
proceed to changing the size of the orifice cap. The size should A2.6.4 If oil is spilled on the outside insulation of the
be changed in increments of 0.001, with each change corre- reaction flask bottom, immediately rinse the oil off with a
sponding to a directly related change of 0.3 % evaporation loss. suitable hydrocarbon solvent. Exercise care not to spread the
The orifice chosen should be of the smallest size giving oil to other areas of the insulation. When all oil has been
accurate results. Rerun the test on the reference fluid after removed, dry the reaction flask bottom with an air source. The
making any changes. flask should be allowed to completely dry at room temperature
NOTE A2.4—If using new glassware, or approximate orifice size is before continuing with the test procedure.
unknown, begin with an 0.084 orifice and increase until good results are
achieved. A2.6.5 Place 10 mL of a varnish removing solvent into the
A2.4.33 If problems persist, contact the instrument manu- reaction flask bottom. Insert clean paper towel into the solvent
facturer. and wipe inside of flask thoroughly, removing any varnish that
may be present on the wall. Rinse carefully with hot water and
A2.4.34 In addition to the procedures described above, dry.
TMC calibration of the instrument is required for results used
in API licensing of automotive engine oils. The calibration A2.6.6 If other glass parts develop a varnish film, clean
procedure is defined in the Lubricant Test Monitoring System these with the same procedure as indicated in A2.6.5 or put the
(LTMS) document that is maintained by the ASTM Test parts into a half/half water or full-strength solution of varnish
Monitoring Center (TMC) and is governed by the D02.B0.07 remover overnight.
Volatility Surveillance Panel. LTMS severity adjustments shall A2.6.7 With a towel dampened with varnish removing
be applied to results used in API licensing of automotive solvent, clean the end of the thermocouple. Wipe with towel
engine oils (A2.7.1.1). dampened with hot water and dry to remove any remaining
cleaning solvent.
A2.5 Sample Procedure
A2.5.1 Perform steps A2.4.4 – A2.4.28 substituting a test A2.7 Calculation
sample for the reference fluid. A2.7.1 Percent volatility is determined by mass loss found
A2.5.2 Calculate the percent evaporation loss of the test by subtracting the combined weight of the flask bottom and oil
sample to the nearest 0.1 %. after testing (see A2.4.27) from their combined weight before
A2.5.3 Collect the volatilized oil (if desired for further the test (see A2.4.4 and A2.4.5).
analysis) from the coalescing filter by placing a small container NOTE A2.7—The percent volatility is obtained by taking the mass loss
under the filter petcock and opening it to release the oil. of the reaction flask and dividing that by the exact mass of the test oil

20
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D5800 − 21
sample recorded earlier: that is, if weight of the oil sample is 65.1 g and However, no comparative data is available for the basestocks.
weight of the oil lost is 10.2 g, then (10.2 g ⁄65.1 g) × 100 = 15.67 %. Further work is necessary to quantitate the relationship.
A2.7.1.1 When results are utilized for API licensing of
automotive engine oils, a severity adjustment (SA) shall be A2.9 Precision8
added to the final calculation of percent volatility. The severity NOTE A2.9—Equipment available from Tannas Co., Michigan U.S.A.,
adjustment is determined from the TMC calibration procedure, was used to develop the precision statement for Procedure C.
as stated in A2.4.34. A2.9.1 The interlaboratory study included ten oils, three
A2.7.2 The mass of volatiles collected is obtained by base oils, and seven finished oils, tested in thirty laboratories.
subtracting the coalescing filter assembly weight before the test
(see A2.4.10) from its weight at the end of the test (see A2.9.2 Repeatability—The quantitative expression for the
A2.4.26). random error associated with the difference between two
independent results obtained under repeatability conditions
NOTE A2.8—The percent of volatiles collected is obtained by dividing
the mass of volatiles collected by the mass loss: that is, if the weight of the that would be exceeded with an approximate probability of 5 %
empty coalescing filter assembly is 163.2 g and the weight of the filter (one case in 20 in the long run) in the normal and correct
assembly after volatilization gained 9.8 g, and if the weight loss shown by operation of the test method:
A2.7.1 is 10.2 g, then (9.8 g ⁄10.2 g) × 100 = 96.08 % of the volatiles were
collected. Repeatability 5 0.1331· X 0.7443 (A2.1)
A2.8 Report A2.9.3 Reproducibility—A quantitative expression for the

random error associated with the difference between two
A2.8.1 Report the evaporation loss to the nearest 0.1 %.
A2.8.1.1 If a severity adjustment is applicable to the result, independent results obtained under reproducibility conditions
the non-adjusted value, the severity adjustment, and the that would be exceeded with an approximate probability of 5 %
severity-adjusted value are to be reported. (one case in 20 in the long run) in the normal and correct
A2.8.2 Limited amount of data available shows that Proce-
dures A and C give similar results for formulated engine oils. Reproducibility 5 0.2411·X 0.7443 (A2.2)
APPENDIXES
(Nonmandatory Information)
X1. HELPFUL HINTS FOR NOACK VOLATILITY (PROCEDURES A and B)
X1.1 Be sure to use the correct manometer fluid to fill the X1.6 There is a drop in metal bath temperature when
manometer. The density of the fluid is critical and must be of inserting the sample. Monitor that the temperature recovers in
the type designed for the manometer (see A1.1.11, Note A1.1). approximately 3 min.
Millimetres of water (implicitly at 1 G) is a unit of pressure.
X1.7 Strong air drafts or turbulence around the pressure
Not every manometer that gives readings in millimetres of
transducer or the heated crucible may adversely affect the test
water is made for use with water as the manometer fluid.
precision and accuracy. Do not place the apparatus in a draft
Consult the manual or manufacturer for the correct manometer
area; however, the exhaust fumes from the evaporating oil shall
fluid properties.
be ventilated to an outside source.
X1.2 Be sure that the manometer reservoir is filled so that X1.8 Clean the crucible and the cover thoroughly with
the manometer is reading exactly zero with no external vacuum solvent between tests and allow to dry. Remove stubborn
or pressure. This should be checked before each run. Evapo- lacquer by immersing in hot detergent solution, by light
ration may require occasional refilling of the manometer abrasion with fine carborundum powder, or a fine abrasive pad.
reservoir. It is also important that the unit be properly leveled.
X1.9 Vacuum must be accurately set and maintained or the
X1.3 For inclined manometers, be sure to read the meniscus Noack values can be greatly altered. Run the pump for 30 min
at the same position at both 1 mm and 20 mm of water. before testing. Vacuum pump should be cleaned out daily using
a hydrocarbon solvent (consult manufacturer for a compatible
X1.4 Rubber tubes used for connections should be changed solvent recommendation). Run a pressure test daily; let the
periodically because oil-mist causes rubber swelling after vacuum run until the pressure stabilizes.
extended period of service. X1.10 Condensed liquid collecting in tubes and at junctions
is also a common source of problem.
X1.5 Cleaning at regular intervals of foreign material ad-
hering on exhaust system parts, particularly on Y-glass piece, is X1.11 It is recommended that a certified Noack reference oil
necessary. check, such as NCO-12, be run each day of operation. Switch

21
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D5800 − 21
the instrument on a minimum of 30 minutes before running the holder to hold the crucible may help prevent splashing while
test to allow temperature stabilization of measurement cir- operating the crucible (see 10.8).
cuitry. X1.19.1 Do not overtighten the crucible lid, and do not use
the extraction tube as a handle to tighten or open the lid.
X1.12 Cleanliness of the extraction tube, glass and silicone
tubing, and air jets should be ensured prior to all tests. X1.20 Timing—Place the crucible in the bath, connect the
vacuum and start timer in quick succession, as nearly simul-
X1.13 Possible contamination of the thermal sensor well taneously as possible.
with slag and Woods metal should be monitored. Slag should
be checked and removed periodically after a series of runs. X1.21 Start the pump before starting the stopwatch for the
test. Instrument electronics must be on for at least 30 min prior
X1.14 Check all connections to be sure they are tight before to the start of the first test to warm up the vacuum transducer.
test. Alignment of all connections without any restrictions Leaving the electronics on overnight satisfies this recommen-
should be maintained. All tubing should allow all flow to travel dation.
downhill to the vacuum pump (no low points).
X1.22 Monitor calibration thermometer versus recorded
X1.15 Verify that the temperature probe holder spring is temperature occasionally during run. The temperature circuit
working properly to seat the probe correctly. The temperature electronics should be verified at least monthly using a cali-
probe should be cleaned to remove varnish. brated temperature probe simulator.
X1.16 On automatic machines, if pressure reads different X1.23 End of Test—Disconnect vacuum at the end of the
from zero before testing, recalibrate the pressure. test time and place the crucible in cooling bath within 1 min.
X1.24 Be careful not to tilt the crucible in handling during
X1.17 If extraction tube is loose, tighten or check the
the test, particularly at the end.
gasket.
X1.25 Final weighing should not be done until the crucible
X1.18 Woods metal bath must be full and overflowing is at room temperature. Do not use extra force (for example,
around crucible and thermal sensor wells. hammers) to open or close the crucible.
X1.19 At all times while handling the sample crucible, be X1.26 At the end of the test, check the pressure and
careful not to splash the test sample on the crucible lid, temperature scans from automatic machines to see that proper
especially when removing the lid. Use of a table-mounted parameters were maintained during the runs.
X2. HELPFUL HINTS FOR SELBY-NOACK VOLATILITY (PROCEDURE C)
X2.1 Be sure that the thermocouple is touching the side of X2.4 For accurate results, make certain that the test runs as
the reaction flask bottom. This can be accomplished by looking close to 1 h as possible (within 15 s).
down through the reaction flask top when positioning the
thermocouple. X2.5 At the end of the test, the glassware may be removed
for the 20 min cool-down period using thermal gloves. This
X2.2 To reduce potential flow problems, make certain that permits immediate starting of another run with a second set of
the hose from the unit to the exhaust hood or vent is not glassware.
pinched anywhere.
X2.3 To prevent leaks, securely seat all glassware, the X2.6 Alternatively, two sets of top and bottom flasks may be
thermocouple sheath, and the orifice tube. used each with its own orifice tube and cap.

22
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D5800 − 21
X3. DRAFT-DEFLECTOR FOR NOACK INSTRUMENTS USED IN PROCEDURES A AND B
X3.1 It is critical to have a draft-free environment for fitted to top of the heating block with its length and width
operating a Noack instrument in the laboratory. The accessory somewhat larger than the dimensions of the top of the heating
described in X3.1 seems to be able to ensure safety as well as block. The box has slots in the sides to allow for protruding
a draft-free environment, since these instruments should be outlet tubes and temperature sensor wires and a hole in the top
operated in a hood. The device isolates the instruments’ heater to allow heat escape.
block environment using a metal box, thus greatly reducing the
air flow immediately around the sample while allowing suffi- X3.3 A diagram of the general form of the accessory is
cient thermal exchange. shown in Fig. X3.1. Different instrument models may require
X3.2 The accessory for instruments used in Procedures A slightly different dimensions in practice.
and B can be made from a 14 GA aluminum sheet for a box

23
'RZQORDGHGSULQWHGE\
D5800 − 21
NOTE 1—Fabricate enclosure to dimensions shown to suit.

NOTE 2—Enclosure material to be 14 GA aluminum.
NOTE 3—Handles and 3⁄4 in. angles to be riveted in place.
FIG. X3.1 Rest Apparatus Top Cover

24
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D5800 − 21
X4. ASTM TEST MONITORING CENTER5 (TMC) CALIBRATION AND SEVERITY ADJUSTMENT FOR AUTO
MOTIVE ENGINE OILS IN PROCEDURES B AND C
X4.1 For percent volatility results used in API licensing of cally similar to those obtained by other laboratories.
automotive engine oils, TMC calibration of instrument is
required. X4.3 This test method is written for use by laboratories that
utilize a section of this test that refer to TMC services.
X4.2 TMC provides reference oils and assesses the test
Laboratories that choose not to use the TMC services may
results obtained on these oils by the laboratory. This allows the
simply ignore these sections.
laboratory to determine if the test method results are statisti-
SUMMARY OF CHANGES
Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D5800 – 20) that may impact the use of this standard. (Approved Oct. 1, 2021.)
(1) Revised subsection 7.2.
Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D5800 – 19a) that may impact the use of this standard. (Approved May 1, 2020.)
(1) Revised subsections 7.2, 10.1, 19.1, and A1.2.2.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
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Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

25
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Evaporation Loss of Lubricating Oils by The Noack Method: Standard Test Method For

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Evaporation Loss of Lubricating Oils by The Noack Method: Standard Test Method For

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

Standard Test Method for

1. Scope* D4057 Practice for Manual Sampling of Petroleum and

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

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FIG. 3 Crucible with Temperature Probe

6.8 Vacuum Pump.

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FIG. 5 Crucible Cover (continued)

6.10 Printer, to print the graphs of the specimen temperature

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FIG. 5 Crucible Cover (continued)

7. Reagents and Materials

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10.4 Run the ball bearing through the extraction tube to

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where: 3 Value by Noack Procedure B⁄D(4)

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FIG. 9 Noack S2 Test Equipment

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A1. PROCEDURE A—WOODS METAL APPARATUS

A1.1 Apparatus The thermometer should be calibrated with appropriate proce-

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NOTE 1—All dimensions in millilitres.

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NOTE 1—All dimensions in millilitres.

A1.1.15 Silicone Rubber Tubing, cut to size, with an inter-

A1.2 Reagents and Materials

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FIG. A1.5 Test Apparatus

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A2. PROCEDURE C—SELBY-NOACK VOLATILITY TEST

A2.1 Apparatus9 A2.1.1.10 Measuring Rod, of known length.

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FIG. A2.1 Selby-Noack Test Equipment

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A2.8 Report A2.9.3 Reproducibility—A quantitative expression for the

X1. HELPFUL HINTS FOR NOACK VOLATILITY (PROCEDURES A and B)

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X2. HELPFUL HINTS FOR SELBY-NOACK VOLATILITY (PROCEDURE C)

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X3. DRAFT-DEFLECTOR FOR NOACK INSTRUMENTS USED IN PROCEDURES A AND B

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NOTE 1—Fabricate enclosure to dimensions shown to suit.

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(1) Revised subsection 7.2.

(1) Revised subsections 7.2, 10.1, 19.1, and A1.2.2.

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&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07