Evaporation Loss of Lubricating Oils by The Noack Method: Standard Test Method For
Evaporation Loss of Lubricating Oils by The Noack Method: Standard Test Method For
Evaporation Loss of Lubricating Oils by The Noack Method: Standard Test Method For
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5800 − 21
FIG. 1 Model A
FIG. 2 Model B
FIG. 7 Extraction Tube (Stainless Steel) with Its Seal (Details 3 and 4 of Fig. 3)
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.
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)
A1.5.7 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
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.
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.
APPENDIXES
(Nonmandatory Information)
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
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.
X2.1 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.
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
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.)
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.)
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