ASTM D5800-14e1
(Test 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
SIGNIFICANCE AND USE
5.1 The evaporation loss is of particular importance in engine lubrication. Where high temperatures occur, portions of an oil can evaporate.
5.2 Evaporation may contribute to oil consumption in an engine and can lead to a change in the properties of an oil.
5.3 Many engine manufacturers specify a maximum allowable evaporation loss.
5.4 Some engine manufacturers, when specifying a maximum allowable evaporation loss, quote this test method along with the specifications.
5.5 Procedure C, using the Selby-Noack apparatus, also permits collection of the volatile oil vapors for determination of their physical and chemical properties. Elemental analysis of the collected volatiles may be helpful in identifying components such as phosphorous, which has been linked to premature degradation of the emission system catalyst.
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-Woods 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 Noack results determined using Procedures A and B show consistent differences. Procedure A gives slightly lower results versus Procedure B on formulated engine oils, while Procedure A gives higher results versus Procedure B on basestocks.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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´1
Designation: D5800 − 14
StandardTest Method for
Evaporation Loss of Lubricating Oils by the Noack Method
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Eq 11 was corrected editorially in January 2015.
1. Scope* Measurement System Performance
D6300Practice for Determination of Precision and Bias
1.1 This test method covers three procedures for determin-
Data for Use in Test Methods for Petroleum Products and
ing the evaporation loss of lubricating oils (particularly engine
Lubricants
oils). Procedure A uses the Noack evaporative tester equip-
2.2 DIN Standards:
ment; Procedure B uses the automated non-Woods metal
DIN 1725Specification for Aluminum Alloys
Noack evaporative apparatus; and Procedure C uses Selby-
DIN 12785Specifications for Glass Thermometers
Noack volatility test equipment.The test method relates to one
set of operating conditions but may be readily adapted to other
3. Terminology
conditions when required.
3.1 Definitions of Terms Specific to This Standard:
1.2 Noack results determined using Procedures A and B
3.1.1 evaporation loss—of a lubricating oil by the Noack
show consistent differences. Procedure A gives slightly lower
method, that mass of volatile oil vapors lost when the oil is
results versus Procedure B on formulated engine oils, while
heatedinatestcruciblethroughwhichaconstantflowofairis
Procedure A gives higher results versus Procedure B on
drawn.
basestocks.
3.1.2 volatility, n—the tendency of a liquid to form a vapor.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 A measured quantity of sample is placed in an evapo-
1.4 This standard does not purport to address all of the
ration crucible or reaction flask that is then heated to 250°C
safety concerns, if any, associated with its use. It is the
with a constant flow of air drawn through it for 60 min. The
responsibility of the user of this standard to establish appro-
loss in mass of the oil is determined.
priate safety and health practices and determine the applica-
4.2 Interlaboratory tests have shown that Procedure A,
bility of regulatory limitations prior to use.
Procedure B, and Procedure C yield essentially equivalent
results, with a correlation coefficient of R = 0.996. See the
2. Referenced Documents
research report for the Selby-Noack interlaboratory study.
2.1 ASTM Standards:
D4057Practice for Manual Sampling of Petroleum and
5. Significance and Use
Petroleum Products
5.1 The evaporation loss is of particular importance in
D4177Practice for Automatic Sampling of Petroleum and
engine lubrication.Where high temperatures occur, portions of
Petroleum Products
an oil can evaporate.
D6299Practice for Applying Statistical Quality Assurance
5.2 Evaporation may contribute to oil consumption in an
and Control Charting Techniques to Evaluate Analytical
engine and can lead to a change in the properties of an oil.
5.3 Many engine manufacturers specify a maximum allow-
This test method is under the jurisdiction of ASTM Committee D02 on
able evaporation loss.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
5.4 Some engine manufacturers, when specifying a maxi-
Current edition approved Oct. 1, 2014. Published October 2014. Originally
mum allowable evaporation loss, quote this test method along
approved in 1995. Last previous edition approved in 2008 as D5800–10. DOI:
with the specifications.
10.1520/D5800-14E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available from Deutsches Institut für Normunge, Beuth Verlag GmbH, Burg-
the ASTM website. grafen Strasse 6, 1000 Berlin 30, Germany.
*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
´1
D5800 − 14
5.5 Procedure C, using the Selby-Noack apparatus, also 6.10 Two Glass Bottles, approximately 2-L capacity, fitted
permits collection of the volatile oil vapors for determination with rubber bungs bored to receive inlet and outlet tubes (see
oftheirphysicalandchemicalproperties.Elementalanalysisof Fig. 4).
the collected volatiles may be helpful in identifying compo-
6.11 Manometer, inclined form, water-filled, precision 0.2
nentssuchasphosphorous,whichhasbeenlinkedtopremature
mm H O or suitable pressure sensor capable of measuring 20
degradation of the emission system catalyst.
6 0.2 mm of H O (a 0 to 50-mm H O pressure transducer has
2 2
been found to be satisfactory).
Procedure A
NOTE1—Somemanometersusewaterasthereferencefluid,othersmay
use a lower density fluid correlated to read in millimetres of water. Users
should ensure that the manometer is filled with the correct density
6. Apparatus
reference fluid.
6.1 Noack Evaporative Tester, comprising the following:
6.12 Glass T-Piece, with bleed valve attached.
6.1.1 Electrically Heated Block Unit, made from a mal-
6.13 Vacuum Pump.
leablealuminumalloy(seeDIN1725,Sheet1),insulatedatthe
jacket and base against loss of heat. (Warning—This block is
6.14 Timer, with accuracy of 0.2 s.
heatedto250°C.)Theblockisheatedelectricallybyabaseand
6.15 Silicone Rubber Tubing, cut to size, with an internal
jacketheater,havingatotalpowerconsumptionof1to1.2kW.
diameter of 4 mm.
In this respect the difference between both individual power
6.15.1 40-mm long; three pieces required,
consumption should not exceed 0.15 kW. In the center of the
6.15.2 300-mm long, and
heatingblock,thereisacircularrecesstoinserttheevaporating
6.15.3 100-mm long.
crucible,thespacebetweenblockandcruciblebeingfilledwith
NOTE 2—The use of automated equipment is permissible as long as it
Woodsalloyorasuitableequivalent.Twocatchesontheblock
gives equivalent results specified in this test method. All hardware
prevent the crucible from rising in the liquid metal bath. Two
dimensions, make-up of the block, crucible, heat capacity, and so forth,
additionalcircularrecessesatequalintervalsfromthecenterof
and glassware must conform to the specifications given in this test
the block are provided for the thermometers (see Fig. 1).
method.
6.1.2 Evaporating Crucible, with screw cover. The crucible
7. Reagents and Materials
is made of stainless steel (see Fig. 2). Above the support ring
is the thread for the cover. The nickel-plated brass cover is
7.1 Cleaning Solvent—Amixture of naphtha and toluene is
hermetically sealed to the crucible by an internal conical
recommended for the cleaning of the crucible. (Warning—
sealing surface (see Fig. 3). Three nozzles of hardened steel
Flammable, vapor harmful.) Overnight soaking may be neces-
permit the air stream to pass through the cover. The extraction
sary.
tube,whichslopesdownward,leadsfromathreadedandsealed
7.2 Oils having a known evaporative loss, the value of
connection in the center of the cover.
which is provided by the oil supplier. Some examples of such
6.2 Balance, capable of weighing at least 200 g to the
oils include RL-N, RL 172, and RL 223, supplied by CEC.
nearest 0.01 g.
Other oils supplied by other vendors may also be used.
6.3 Crucible Clamp and Spanner. 7.3 Insulated Gloves.
7.4 Paint Brush,suchasatinnerpsacidbrush(15to25-mm
6.4 Reamer, 2-mm diameter.
width).
6.5 Ball Bearing, 3.5-mm diameter.
7.5 Woods Metal or Suitable Heat Transfer Material—
6.6 Thermometer, M260 (see DIN 12785) or temperature
(Warning—Woods metal contains lead (25 %), bismuth
sensing device capable of reading temperature to 0.1°C. The
(50%),antimony(12.5%),andcadmium(12.5%);thesehave
thermometer should be calibrated with appropriate procedure
been found to be health hazardous.Avoid contact with skin at
at appropriate frequency (generally every six months).
all times.)
6.7 Contact Type Control Thermometer (for manual).
8. Hazards
6.8 GlassY-piece,aninternaldiameterof4mm.Theupright
8.1 Safety Hazards—It is assumed that anyone using this
arms,each45-mmlong,shouldformananglesuchthatthearm
test method will either be fully trained and familiar with all
connected to the crucible extraction tube and theY-piece form
normal laboratory practices, or will be under the direct super-
a straight line. The vertical arm is 60-mm long and beveled at
vision of such a person. It is the responsibility of the operator
45°.
to ensure that all local legislative and statutory requirements
6.9 Glass Delivery Tubes, an internal diameter of 4 mm,
are met.
each arm length 100 mm, beveled at 45° at ends entering and
leaving the bottles.
6.9.1 Bent at an angle of approximately 80°. The sole source of supply ofWoods metal known to the committee at this time
is Sigma-Aldrich, Customer Support, P.O. Box 14508, St. Louis, MO 63178. If you
6.9.2 Bent at an angle of approximately 100°, length to 20
are aware of alternative suppliers, please provide this information to ASTM
mm of bottle base.
International Headquarters. Your comments will receive careful consideration at a
6.9.3 Bent at an angle of approximately 90°. meeting of the responsible technical committee, which you may attend.
´1
D5800 − 14
NOTE 1—All dimensions in millilitres.
FIG. 1 Heating Block
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D5800 − 14
NOTE 1—All dimensions in millilitres.
NOTE 1—All dimensions in millilitres.
FIG. 2 Crucible
FIG. 3 Cover
8.2 (Warning—Though the test method calls for a draft-
–free area, the exhaust fumes from the evaporating oil must be
supplied to the heating block so that the temperature can be
ventilated to an outside source. Precaution shall be taken to
maintained at 250 6 0.5°C.
avoid any possibility of fire or explosion.)
NOTE 3—One way to achieve a draft–free environment and greater
9.4 Assemble the remaining apparatus, less the crucible, as
safetyinoperationfortheinstrumentsusedinthistestmethodisdescribed
shown in Fig. 5.
in Appendix X3.
9.5 Place an empty crucible in the heating block, securing
8.3 An alternate means for preventing draft described in
the flange under the screw heads against the buoyancy of the
Appendix X3 was not used in the development of the test
Woodsmetal.Thelevelofthemoltenmetalshouldbesuchthat
method precision statement.
atraceofitcanbeseenattheflangeofthecrucibleandthetop
9. Preparation of Apparatus of the heating block.
9.1 AstandardassemblyoftheapparatusisshowninFig.5.
9.6 Check that the readings can be obtained on the manom-
To avoid disturbing the thermal equilibrium, the apparatus
eter scale, or other measuring device, by connecting the
shall be assembled in a draft–free area and comply with Fig. 5
crucible to the assembled apparatus. A reading of 20.0 6 0.2
in dimensions and apparatus. (See 8.2.)
mm shall be obtained.
9.2 AddsufficientWoodsmetalorequivalentmaterialtothe
9.7 Disconnectandremovethecruciblefromtheassembled
recesses of the heating block so that, with the crucible and
apparatus.
thermometer in place, the remaining spaces will be filled with
9.8 Switch off the pump and the heating block and raise the
the molten metal.
crucible and the thermometers from the molten Woods metal.
9.3 Using the highest heating rate possible, raise the tem-
Using the brush, return any Woods metal clinging to the
perature of the heating block until the Woods metal is molten.
crucible to the heating block.
Insertthethermometerswiththeirbulbstouchingthebottomof
the recesses, and ensure that the contact thermometer is 9.9 Clean theY-piece and glass tubing to prevent a build up
plugged in the back of the heating block. Adjust the power of condensate.
´1
D5800 − 14
at the bottom of the heating block recess. The heating block and the
thermometerrecessesshouldbecleanedandtheWoodsmetalreplacedon
a regular basis to avoid the accumulation of slag. Oxidized Woods metal
will affect the heat transfer to the crucible and hence may have a
deleterious effect on the results obtained.
10.9 Adjust the control on the heating block to maintain the
block temperature approximately 5°C below the test tempera-
ture. Readjust the temperature control so that the test tempera-
ture is reestablished within 3 min of the start of the test.
NOTE 5—Temperature and pressure will be controlled automatically
when automated equipment is used.
10.10 Atthestartofthetest,constantattentionshallbepaid
to maintaining the correct pressure. Once this becomes steady,
usually within 10 to 15 min, check periodically that the
temperature and pressure differential remain constant through-
out the period of the test.
10.11 After 60 min 6 5 s, lift the crucible from the heating
block, remove any adhering alloy, and place the crucible in a
warm water bath to a depth of at least 30 mm.The time period
from the end of the test to immersion of the crucible shall not
exceed 60 s.
10.12 After30min,removethecruciblefromthewater,dry
FIG. 4 Glassware
the outside, and carefully remove the lid.
10.13 Reweigh the crucible without the lid to the nearest
10. Verification
0.01 g.
10.1 Switch on the pump and the heating block and ensure
10.14 Calculate to the nearest 0.1% mass/mass (M/M) the
that the apparatus is assembled, minus the crucible, as shown
evaporation loss of the reference oil.
in Fig. 5.
10.15 Compare the result obtained against the given value
10.2 Checkthatthecrucibleandcoverarefreefromlacquer.
for the reference oil. If the result is within 6% of the value,
10.2.1 After every test, clean the crucible and cover with
repeat the procedure from 11.1, using the test sample.
solvent and allow to dry. Stubborn lacquer can be cleaned by
abrasion from a glass beader under pressure.
10.16 If the result is not within 6% of the given value,
check that the apparatus complies with that shown in Fig. 5,
10.3 Passthereamerthrougheachofthethreenozzlesinthe
and that the procedure has been adhered to. Check the
covertoensurethattheyareclear.(Warning—Usingareamer
calibration of the thermometer and pressure sensing device.
withadiameterlargerthan2mmcanenlargethenozzles.This
can lead to higher losses because of increased air flow.)
10.17 Re-check the evaporation loss of the reference oil.
10.4 Run the ball bearing through the extraction tube to
NOTE6—Condensateshouldnotbeallowedto
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D5800 − 14 D5800 − 14
Standard Test Method for
Evaporation Loss of Lubricating Oils by the Noack Method
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.
ε NOTE—Eq 11 was corrected editorially in January 2015.
1. 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-Woods 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 Noack results determined using Procedures A and B show consistent differences. Procedure A gives slightly lower results
versus Procedure B on formulated engine oils, while Procedure A gives higher results versus Procedure B on basestocks.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
2.2 DIN Standards:
DIN 1725 Specification for Aluminum Alloys
DIN 12785 Specifications for Glass Thermometers
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 evaporation loss—of a lubricating oil by the Noack method, that mass of volatile oil vapors lost when the oil is heated
in a test crucible through which a constant flow of air is drawn.
3.1.2 volatility, n—the tendency of a liquid to form a vapor.
4. Summary of Test Method
4.1 A measured quantity of sample is placed in an evaporation crucible or reaction flask that is then heated to 250°C with a
constant flow of air drawn through it for 60 min. The loss in mass of the oil is determined.
4.2 Interlaboratory tests have shown that Procedure A, Procedure B, and Procedure C yield essentially equivalent results, with
a correlation coefficient of R = 0.996. See the research report for the Selby-Noack interlaboratory study.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.06 on Analysis of Liquid Fuels and Lubricants.
Current edition approved Oct. 1, 2014. Published October 2014. Originally approved in 1995. Last previous edition approved in 2008 as D5800 – 10. DOI:
10.1520/D5800-14.10.1520/D5800-14E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from Deutsches Institut für Normunge, Beuth Verlag GmbH, Burggrafen Strasse 6, 1000 Berlin 30, Germany.
*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
´1
D5800 − 14
5. Significance and Use
5.1 The evaporation loss is of particular importance in engine lubrication. Where high temperatures occur, portions of an oil can
evaporate.
5.2 Evaporation may contribute to oil consumption in an engine and can lead to a change in the properties of an oil.
5.3 Many engine manufacturers specify a maximum allowable evaporation loss.
5.4 Some engine manufacturers, when specifying a maximum allowable evaporation loss, quote this test method along with the
specifications.
5.5 Procedure C, using the Selby-Noack apparatus, also permits collection of the volatile oil vapors for determination of their
physical and chemical properties. Elemental analysis of the collected volatiles may be helpful in identifying components such as
phosphorous, which has been linked to premature degradation of the emission system catalyst.
Procedure A
6. Apparatus
6.1 Noack Evaporative Tester, comprising the following:
6.1.1 Electrically Heated Block Unit, made from a malleable aluminum alloy (see DIN 1725, Sheet 1), insulated at the jacket
and base against loss of heat. (Warning—This block is heated to 250°C.) The block is heated electrically by a base and jacket
heater, having a total power consumption of 1 to 1.2 kW. In this respect the difference between both individual power consumption
should not exceed 0.15 kW. In the center of the heating block, there is a circular recess to insert the evaporating crucible, the space
between block and crucible being filled with Woods alloy or a suitable equivalent. Two catches on the block prevent the crucible
from rising in the liquid metal bath. Two additional circular recesses at equal intervals from the center of the block are provided
for the thermometers (see Fig. 1).
6.1.2 Evaporating Crucible, with screw cover. The crucible is made of stainless steel (see Fig. 2). Above the support ring is the
thread for the cover. The nickel-plated brass cover is hermetically sealed to the crucible by an internal conical sealing surface (see
Fig. 3). Three nozzles of hardened steel permit the air stream to pass through the cover. The extraction tube, which slopes
downward, leads from a threaded and sealed connection in the center of the cover.
6.2 Balance, capable of weighing at least 200 g to the nearest 0.01 g.
6.3 Crucible Clamp and Spanner.
6.4 Reamer, 2-mm diameter.
6.5 Ball Bearing, 3.5-mm diameter.
6.6 Thermometer, M260 (see DIN 12785) or temperature sensing device capable of reading temperature to 0.1°C. The
thermometer should be calibrated with appropriate procedure at appropriate frequency (generally every six months).
6.7 Contact Type Control Thermometer (for manual).
6.8 Glass Y-piece, an internal diameter of 4 mm. The upright arms, each 45-mm long, should form an angle such that the arm
connected to the crucible extraction tube and the Y-piece form a straight line. The vertical arm is 60-mm long and beveled at 45°.
6.9 Glass Delivery Tubes, an internal diameter of 4 mm, each arm length 100 mm, beveled at 45° at ends entering and leaving
the bottles.
6.9.1 Bent at an angle of approximately 80°.
6.9.2 Bent at an angle of approximately 100°, length to 20 mm of bottle base.
6.9.3 Bent at an angle of approximately 90°.
6.10 Two Glass Bottles, approximately 2-L capacity, fitted with rubber bungs bored to receive inlet and outlet tubes (see Fig.
4).
6.11 Manometer, inclined form, water-filled, precision 0.2 mm H O or suitable pressure sensor capable of measuring 20 6 0.2
mm of H O (a 0 to 50-mm H O pressure transducer has been found to be satisfactory).
2 2
NOTE 1—Some manometers use water as the reference fluid, others may use a lower density fluid correlated to read in millimetres of water. Users
should ensure that the manometer is filled with the correct density reference fluid.
6.12 Glass T-Piece, with bleed valve attached.
6.13 Vacuum Pump.
6.14 Timer, with accuracy of 0.2 s.
6.15 Silicone Rubber Tubing, cut to size, with an internal diameter of 4 mm.
6.15.1 40-mm long; three pieces required,
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D5800 − 14
NOTE 1—All dimensions in millilitres.
FIG. 1 Heating Block
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D5800 − 14
NOTE 1—All dimensions in millilitres.
FIG. 2 Crucible
6.15.2 300-mm long, and
6.15.3 100-mm long.
NOTE 2—The use of automated equipment is permissible as long as it gives equivalent results specified in this test method. All hardware dimensions,
make-up of the block, crucible, heat capacity, and so forth, and glassware must conform to the specifications given in this test method.
7. Reagents and Materials
7.1 Cleaning Solvent—A mixture of naphtha and toluene is recommended for the cleaning of the crucible. (Warning—
Flammable, vapor harmful.) Overnight soaking may be necessary.
7.2 Oils having a known evaporative loss, the value of which is provided by the oil supplier. Some examples of such oils include
RL-N, RL 172, and RL 223, supplied by CEC. Other oils supplied by other vendors may also be used.
7.3 Insulated Gloves.
7.4 Paint Brush, such as a tinnerps acid brush (15 to 25-mm width).
7.5 Woods Metal or Suitable Heat Transfer Material—(Warning—Woods metal contains lead (25 %), bismuth (50 %),
antimony (12.5 %), and cadmium (12.5 %); these have been found to be health hazardous. Avoid contact with skin at all times.)
8. Hazards
8.1 Safety Hazards—It is assumed that anyone using this test method will either be fully trained and familiar with all normal
laboratory practices, or will be under the direct supervision of such a person. It is the responsibility of the operator to ensure that
all local legislative and statutory requirements are met.
The sole source of supply of Woods metal known to the committee at this time is Sigma-Aldrich, Customer Support, P.O. Box 14508, St. Louis, MO 63178. If you are
aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend.
´1
D5800 − 14
NOTE 1—All dimensions in millilitres.
FIG. 3 Cover
FIG. 4 Glassware
´1
D5800 − 14
FIG. 5 Test Apparatus
8.2 (Warning—Though the test method calls for a draft–free area, the exhaust fumes from the evaporating oil must be
ventilated to an outside source. Precaution shall be taken to avoid any possibility of fire or explosion.)
NOTE 3—One way to achieve a draft–free environment and greater safety in operation for the instruments used in this test method is described in
Appendix X3.
8.3 An alternate means for preventing draft described in Appendix X3 was not used in the development of the test method
precision statement.
9. Preparation of Apparatus
9.1 A standard assembly of the apparatus is shown in Fig. 5. To avoid disturbing the thermal equilibrium, the apparatus shall
be assembled in a draft–free area and comply with Fig. 5 in dimensions and apparatus. (See 8.2.)
9.2 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.
9.3 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 6 0.5°C.
9.4 Assemble the remaining apparatus, less the crucible, as shown in Fig. 5.
9.5 Place an empty crucible in the heating block, securing 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.
9.6 Check that the readings can be obtained on the manometer scale, or other measuring device, by connecting the crucible to
the assembled apparatus. A reading of 20.0 6 0.2 mm shall be obtained.
9.7 Disconnect and remove the crucible from the assembled apparatus.
9.8 Switch off the pump and the heating block and raise the crucible and the thermometers from the molten Woods metal. Using
the brush, return any Woods metal clinging to the crucible to the heating block.
9.9 Clean the Y-piece and glass tubing to prevent a build up of condensate.
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D5800 − 14
10. Verification
10.1 Switch on the pump and the heating block and ensure that the apparatus is assembled, minus the crucible, as shown in Fig.
5.
10.2 Check that the crucible and cover are free from lacquer.
10.2.1 After every test, clean the crucible and cover with solvent and allow to dry. Stubborn lacquer can be cleaned by abrasion
from a glass beader under pressure.
10.3 Pass the reamer through each of the three nozzles in the cover to ensure that they are clear. (Warning—Using a reamer
with a diameter larger than 2 mm can enlarge the nozzles. This can lead to higher losses because of increased air flow.)
10.4 Run the ball bearing through the extraction tube to ensure that it is clear of dirt.
10.5 Weigh the empty crucible without its cover to the nearest 0.01 g.
10.6 Weigh into the crucible 65.0 6 0.1 g of the Reference Oil.
10.7 Screw on the cover using the clamp and spanner.
10.8 Ensure the temperature of the heating block is at 250 6 0.5°C. Place the crucible in its recess in the heating block, securing
the flange under the screw heads against the buoyancy of the Woods metal. Switch the control of the heating block to compensate
for the heat capacity of the crucible. Immediately (in less than 5 s), connect the extraction tube of the crucible to the arm of the
glass Y-piece, making a butt joint. Simultaneously, start the pump and the stopwatch and adjust the bleed valve to give a pressure
differential of 20 6 0.2 mm.
NOTE 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 flange
above the heating block may suggest a buildup of Woods metal 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 a regular basis to avoid the accumulation of slag. Oxidized Woods metal will affect
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