Standard Test Method for Evaporation Loss of Lubricating Oils by the Noack Method

SCOPE
1.1 This test method covers three procedures for determining the evaporation loss of lubricating oils (particularly engine oils). Procedure A uses the Noack evaporative tester equipment; Procedure B uses the automated non-Wood's metal Noack evaporative apparatus, and Procedure C uses Selby-Noack volatility test equipment. The test method relates to one set of operating conditions but may be readily adapted to other conditions when required.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.  See Sections 8 and 18 and 6.1.1, 7.1, 7.5, 9.1, 10.3, and 17.1 for specific precautionary statements.

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09-Aug-2000
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ASTM D5800-00a - Standard Test Method for Evaporation Loss of Lubricating Oils by the Noack Method
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5800 – 00a An American National Standard
Standard Test Method for
Evaporation Loss of Lubricating Oils by the Noack Method
This standard is issued under the fixed designation D 5800; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method covers three procedures for determin- 3.1 Definitions of Terms Specific to This Standard:
ing the evaporation loss of lubricating oils (particularly engine 3.1.1 evaporation loss—of a lubricating oil by the Noack
oils). Procedure A uses the Noack evaporative tester equip- method, that mass of volatile oil vapors lost when the oil is
ment; Procedure B uses the automated non-Wood’s metal heated in a test crucible through which a constant flow of air is
Noack evaporative apparatus, and Procedure C uses Selby- drawn.
Noack volatility test equipment. The test method relates to one 3.1.2 volalitity, n—the tendency of a liquid to form a vapor.
set of operating conditions but may be readily adapted to other
4. Summary of Test Method
conditions when required.
1.2 The values stated in SI units are to be regarded as the 4.1 A measured quantity of sample is placed in an evapo-
ration crucible or reaction flask that is then heated to 250°C
standard. The values given in parentheses are for information
only. with a constant flow of air drawn through it for 60 min. The
loss in mass of the oil is determined.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.2 Interlaboratory tests have shown that Procedure A,
Procedure B, and Procedure C yield essentially equivalent
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- results, with a correlation coefficient of R squared = 0.996. See
research report RR:D02-1462 for the Selby-Noack interlabo-
bility of regulatory limitations prior to use. See Sections 8 and
18 and 6.1.1, 7.1, 7.5, 9.1, 10.3, and 17.1 for specific ratory study.
precautionary statements.
5. Significance and Use
2. Referenced Documents
5.1 The evaporation loss is of particular importance in
engine lubrication. Where high temperatures occur, portions of
2.1 ASTM Standards:
D 4057 Practice for Manual Sampling of Petroleum and an oil can evaporate.
5.2 Evaporation may contribute to oil consumption in an
Petroleum Products
D 4177 Practice for Automatic Sampling of Petroleum and engine and can lead to a change in the properties of an oil.
5.3 Many engine manufacturers specify a maximum allow-
Petroleum Products
D 6299 Practice for Applying Statistical Quality Assurance able evaporation loss.
Techniques to Evaluate Analytical Measurement System 5.4 Some engine manufacturers, when specifying a maxi-
mum allowable evaporation loss, quote this test method along
Performance
D 6300 Practice for Determination of Precision and Bias with the specifications.
5.5 Procedure C, using the Selby-Noack apparatus, also
Data for Use in Test Methods for Petroleum Products and
Lubricants permits collection of the volatile oil vapors for determination
of their physical and chemical properties. Elemental analysis of
2.2 DIN Standards:
DIN 1725 Specification for Aluminum Alloys the collected volatiles may be helpful in identifying compo-
nents such as phosphorous, which has been linked to premature
DIN 12785 Specifications for Glass Thermometers
degradation of the emission system catalyst.
Procedure A
This test method is under the jurisdiction of ASTM Committee D02 on
6. Apparatus
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.06 on Analysis of Lubricants.
6.1 Noack Evaporative Tester, comprising the following:
Current edition approved Aug. 10, 2000. Published October 2000. Originally
6.1.1 Electrically Heated Block Unit, made from a mal-
published as D 5800 – 95. Last previous edition D 5800 – 00.
Annual Book of ASTM Standards, Vol 05.02. leable aluminum alloy (see DIN 1725, Sheet 1), insulated at the
Annual Book of ASTM Standards, Vol 05.04.
jacket and base against loss of heat. (Warning—This block is
Available from Deutsches Institut für Normunge, Beuth Verlag GmbH, Burg-
heated to 250°C.) The block is heated electrically by a base and
grafen Strasse 6, 1000 Berlin 30, Germany.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5800
NOTE 2—The use of automated equipment is permissible as long as it
jacket heater, having a total power consumption of 1 to 1.2 kW.
gives equivalent results specified in this test method. All hardware
In this respect the difference between both individual power
dimensions, make-up of the block, crucible, heat capacity, and so forth,
consumption should not exceed 0.15 kW. In the center of the
and glassware must conform to the specifications given in this test
heating block, there is a circular recess to insert the evaporating
method.
crucible, the space between block and crucible being filled with
Woods alloy or a suitable equivalent. Two catches on the block 7. Reagents and Materials
prevent the crucible from rising in the liquid metal bath. Two
7.1 Cleaning Solvent—A mixture of naphtha and toluene is
additional circular recesses at equal intervals from the center of
recommended for the cleaning of the crucible. (Warning—
the block are provided for the thermometers (see Fig. 1).
Flammable, vapor harmful.) Overnight soaking may be neces-
6.1.2 Evaporating Crucible, with screw cover. The crucible
sary.
is made of stainless steel (see Fig. 2). Above the support ring
7.2 Datum Oil RL 172, (formerly RL-N) Reference Oil.
is the thread for the cover. The nickel-plated brass cover is
7.3 Insulated Gloves.
hermetically sealed to the crucible by an internal conical
7.4 Paint Brush, such as a tinnerps acid brush (15 to 25-mm
sealing surface (see Fig. 3). Three nozzles of hardened steel
width).
permit the air stream to pass through the cover. The extraction 5
7.5 Woods Metal or suitable heat transfer material—
tube, which slopes downward, leads from a threaded and sealed
(Warning—Woods metal contains lead (25 %), bismuth
connection in the center of the cover.
(50 %), antimony (12.5 %), and cadmium (12.5 %); these have
6.2 Balance, capable of weighing at least 200 g to the
been found to be health hazardous. Avoid contact with skin at
nearest 0.01 g.
all times.)
6.3 Crucible Clamp and Spanner.
8. Hazards
6.4 Reamer, 2-mm diameter.
6.5 Ball Bearing, 3.5-mm diameter.
8.1 Safety Hazards—It is assumed that anyone using this
6.6 Thermometer, M260 (see DIN 12785) or temperature test method will either be fully trained and familiar with all
sensing device capable of reading temperature to 0.1°C. The normal laboratory practices, or will be under the direct super-
thermometer should be calibrated with appropriate procedure vision of such a person. It is the responsibility of the operator
at appropriate frequency (generally every six months). to ensure that all local legislative and statutory requirements
6.7 Contact Type Control Thermometer (for manual). are met.
6.8 Glass Y-piece, an internal diameter of 4 mm. The upright 8.2 Warning—Though the test method calls for a draft free
arms, each 45-mm long, should form an angle such that the arm area, the exhaust fumes from the evaporating oil must be
ventilated to an outside source. Precaution shall be taken to
connected to the crucible extraction tube and the Y-piece form
a straight line. The vertical arm is 60-mm long and beveled at avoid any possibility of fire or explosion.
45°.
9. Preparation of Apparatus
6.9 Glass Delivery Tubes, an internal diameter of 4 mm,
9.1 A standard assembly of the apparatus is shown in Fig. 5.
each arm length 100 mm, beveled at 45° at ends entering and
To avoid disturbing the thermal equilibrium, the apparatus
leaving the bottles.
shall be assembled in a draft free area and comply with Fig. 5
6.9.1 Bent at an angle of approximately 80°.
in dimensions and apparatus. (Warning—see 8.2.)
6.9.2 Bent at an angle of approximately 100°, length to 20
9.2 Add sufficient Woods metal or equivalent material to the
mm of bottle base.
recesses of the heating block so that, with the crucible and
6.9.3 Bent at an angle of approximately 90°.
thermometer in place, the remaining spaces will be filled with
6.10 Two Glass Bottles, approximately 2-L capacity, fitted
the molten metal.
with rubber bungs bored to receive inlet and outlet tubes (see
9.3 Using the highest heating rate possible, raise the tem-
Fig. 4).
perature of the heating block until the Woods metal is molten.
6.11 Manometer, inclined form, water-filled, precision 0.2
Insert the thermometers with their bulbs touching the bottom of
mm H O or suitable pressure sensor capable of measuring 20
the recesses, and ensure that the contact thermometer is
6 0.2 mm of H O (a 0 to 50-mm H O pressure transducer has
2 2
plugged in the back of the heating block. Adjust the power
been found to be satisfactory).
supplied to the heating block so that the temperature can be
NOTE 1—Some manometers use water as the reference fluid, others
maintained at 250 6 0.5°C.
may use a lower density fluid correlated to read in millimetres of water.
9.4 Assemble the remaining apparatus, less the crucible, as
Users should ensure that the manometer is filled with the correct density
shown in Fig. 5.
reference fluid.
9.5 Place an empty crucible in the heating block, securing
6.12 Glass T-Piece, with bleed valve attached.
the flange under the screw heads against the buoyancy of the
6.13 Vacuum Pump.
Woods metal. The level of the molten metal should be such that
6.14 Timer, with accuracy of 0.2 s.
a trace of it can be seen at the flange of the crucible and the top
6.15 Silicone Rubber Tubing, cut to size, with an internal
of the heating block.
diameter of 4 mm.
6.15.1 40-mm long; three pieces required,
Woods metal, available from Aldrich Chemical Co., has been found satisfactory
6.15.2 300-mm long, and
for this purpose. An equivalent may be used. Subcommittee D02.06 is evaluating
6.15.3 100-mm long. less toxic alloys as alternatives.
D 5800
NOTE 1—All dimensions in millilitres.
FIG. 1 Heating Block
D 5800
NOTE 1—All dimensions in millilitres.
FIG. 2 Crucible
9.6 Check that the readings can be obtained on the manom- 10.5 Weigh the empty crucible without its cover to the
eter scale, or other measuring device, by connecting the nearest 0.01 g.
crucible to the assembled apparatus. A reading of 20.0 6 0.2
10.6 Weigh into the crucible 65.0 6 0.1 g of the Reference
mm shall be obtained.
Oil.
9.7 Disconnect and remove the crucible from the assembled
10.7 Screw on the cover using the clamp and spanner.
apparatus.
10.8 Ensure the temperature of the heating block is at 250 6
9.8 Switch off the pump and the heating block and raise the
0.5°C. Place the crucible in its recess in the heating block,
crucible and the thermometers from the molten Woods metal.
securing the flange under the screw heads against the buoyancy
Using the brush, return any Woods metal clinging to the
of the Woods metal. Switch the control of the heating block to
crucible to the heating block.
compensate for the heat capacity of the crucible. Immediately
9.9 Clean the Y-piece and glass tubing to prevent a build up
(in less than 5 s), connect the extraction tube of the crucible to
of condensate.
the arm of the glass Y-piece, making a butt joint. Simulta-
10. Verification
neously, start the pump and the stopwatch and adjust the bleed
valve to give a pressure differential of 20 6 0.2 mm.
10.1 Switch on the pump and the heating block and ensure
that the apparatus is assembled, minus the crucible, as shown
NOTE 3—When the crucible is in the test position, its flange should be
in Fig. 5.
flush with the top of the heating block. Any protrusion of the crucible
10.2 Check that the crucible and cover are free from lacquer.
flange above the heating block may suggest a build-up of Woods metal
10.2.1 After every test, clean the crucible and cover with
slag at the bottom of the heating block recess. The heating block and the
thermometer recesses should be cleaned and the Woods metal replaced on
solvent and allow to dry. Stubborn lacquer can be cleaned by
a regular basis to avoid the accumulation of slag. Oxidized Woods metal
abrasion from a glass beader under pressure.
will affect the heat transfer to the crucible and hence may have a
10.3 Pass the reamer through each of the three nozzles in the
deleterious effect on the results obtained.
cover to ensure that they are clear. (Warning—Using a reamer
with a diameter larger than 2 mm can enlarge the nozzles. This 10.9 Adjust the control on the heating block to maintain the
can lead to higher losses because of increased air flow.) block temperature approximately 5°C below the test tempera-
10.4 Run the ball bearing through the extraction tube to ture. Readjust the temperature control so that the test tempera-
ensure that it is clear of dirt. ture is reestablished within 3 min of the start of the test.
D 5800
NOTE 1—All dimensions in millilitres.
FIG. 3 Cover
FIG. 4 Glassware
NOTE 4—Temperature and pressure will be controlled automatically
out the period of the test.
when automated equipment is used.
10.11 After 60 min 65 s, lift the crucible from the heating
10.10 At the start of the test, constant attention shall be paid block, remove any adhering alloy, and place the crucible in a
to maintaining the correct pressure. Once this becomes steady, warm water bath to a depth of at least 30 mm. The time period
usually within 10 to 15 min, check periodically that the from the end of the test to immersion of the crucible shall not
temperature and pressure differential remain constant through- exceed 60 s.
D 5800
FIG. 5 Test Apparatus
10.12 After 30 min, remove the crucible from the water, dry 12. Calculations and Results
the outside, and carefully remove the lid.
12.1 Evaporation loss is obtained from the difference in
10.13 Reweigh the crucible without the lid to the nearest
weight before and after1hat 250°C.
0.01 g.
~B 2 A! 2 ~C 2 A!
10.14 Calculate to the nearest 0.1 % mass/mass (M/M) the
evaporation loss 5 3 100 (1)
B 2 A
evaporation loss of the Reference Oil.
10.15 Compare the result obtained against the given value
where:
for the Reference Oil. If the result i
...

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