ASTM D7873-13(2017)
(Test Method)Standard Test Method for Determination of Oxidation Stability and Insolubles Formation of Inhibited Turbine Oils at 120 °C Without the Inclusion of Water (Dry TOST Method)
Standard Test Method for Determination of Oxidation Stability and Insolubles Formation of Inhibited Turbine Oils at 120 °C Without the Inclusion of Water (Dry TOST Method)
SIGNIFICANCE AND USE
5.1 Insoluble material may form in oils that are subjected to oxidizing conditions.
5.2 Significant formation of oil insolubles or metal corrosion products, or both, during this test may indicate that the oil will form insolubles or corrode metals, or both, resulting in varnish formation during field service. The level of varnish formation in service will be dependent on many factors (turbine design, reservoir temperature, duty-cycle, for example. peaking, cycling, or base-load duty, maintenance, and so forth) and a direct correlation between results in this test and field varnish formation are yet to be established.
5.3 Oxidation condition at 120 °C under accelerated oxidation environment of Test Method D4310 and measurement of sludge and RPVOT value could reflect a practical oil quality in actual turbine operations. Results from this test should be used together with other key lubricant performance indicators (including other established oxidation and corrosion tests) to indicate suitability for service.
SCOPE
1.1 This test method is used to evaluate the sludging tendencies of steam and gas turbine lubricants during the oxidation process in the presence of oxygen and metal catalyst (copper and iron) at an elevated temperature. This test method may be used to evaluate industrial oils (for example, circulating oils and so forth).
1.2 This test method is a modification of Test Method D4310 where the sludging and corrosion tendencies of the same kinds of oils are determined after 1000 h at 95 °C in the presence of water. Water is omitted in this modification.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 Exception—The values in parentheses in some of the figures are provided for information only for those using old equipment based on non-SI units.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website—http://www.epa.gov/mercury/faq.htm—for additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be prohibited by law.
1.6 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.
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Designation: D7873 − 13 (Reapproved 2017)
Standard Test Method for
Determination of Oxidation Stability and Insolubles
Formation of Inhibited Turbine Oils at 120 °C Without the
Inclusion of Water (Dry TOST Method)
This standard is issued under the fixed designation D7873; 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 1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method is used to evaluate the sludging
ization established in the Decision on Principles for the
tendencies of steam and gas turbine lubricants during the
Development of International Standards, Guides and Recom-
oxidation process in the presence of oxygen and metal catalyst
mendations issued by the World Trade Organization Technical
(copper and iron) at an elevated temperature. This test method
Barriers to Trade (TBT) Committee.
may be used to evaluate industrial oils (for example, circulat-
ing oils and so forth).
2. Referenced Documents
1.2 This test method is a modification of Test Method 2
2.1 ASTM Standards:
D4310 where the sludging and corrosion tendencies of the
A510M Specification for General Requirements for Wire
same kinds of oils are determined after 1000 h at 95 °C in the
Rods and Coarse Round Wire, Carbon Steel (Metric)
presence of water. Water is omitted in this modification. 3
(Withdrawn 2011)
1.3 The values stated in SI units are to be regarded as B1 Specification for Hard-Drawn Copper Wire
standard. No other units of measurement are included in this D943 Test Method for Oxidation Characteristics of Inhibited
standard. Mineral Oils
1.3.1 Exception—The values in parentheses in some of the D1193 Specification for Reagent Water
figures are provided for information only for those using old D2272 Test Method for Oxidation Stability of Steam Tur-
equipment based on non-SI units. bine Oils by Rotating Pressure Vessel
D4057 Practice for Manual Sampling of Petroleum and
1.4 This standard does not purport to address all of the
Petroleum Products
safety concerns, if any, associated with its use. It is the
D4310 Test Method for Determination of Sludging and
responsibility of the user of this standard to establish appro-
Corrosion Tendencies of Inhibited Mineral Oils
priate safety, health, and environmental practices and deter-
E1 Specification for ASTM Liquid-in-Glass Thermometers
mine the applicability of regulatory limitations prior to use.
E230/E230M Specification for Temperature-Electromotive
1.5 WARNING—Mercury has been designated by many
Force (emf) Tables for Standardized Thermocouples
regulatory agencies as a hazardous material that can cause
2.2 Other Standards:
central nervous system, kidney and liver damage. Mercury, or
Specification for IP Standard Thermometers
its vapor, may be hazardous to health and corrosive to
ISO 3696 Water for Analytical Laboratory Use—
materials.Cautionshouldbetakenwhenhandlingmercuryand
Specification and Test Methods
mercury containing products. See the applicable product Ma-
terial Safety Data Sheet (MSDS) for details and EPA’s
3. Terminology
website—http://www.epa.gov/mercury/faq.htm—for addi-
3.1 Definitions:
tional information. Users should be aware that selling mercury
and/or mercury containing products into your state or country
may be prohibited by law. 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
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
1 3
This test method is under the jurisdiction of ASTM Committee D02 on The last approved version of this historical standard is referenced on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of www.astm.org.
Subcommittee D02.09.0C on Oxidation of Turbine Oils. Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
Current edition approved Dec. 1, 2017. Published December 2017. Originally U.K., http://www.energyinst.org.
ε2 5
approved in 2013. Last previous edition approved in 2013 as D7873 – 13 . DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D7873-13R17. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7873 − 13 (2017)
3.1.1 sludge, n—a precipitate or sediment from oxidized 6.2.1.1 Use of heated liquid baths that are designed and
mineral oil that is insoluble in n-heptane. constructed of metal, or combinations of metals and other
suitable opaque materials, that prevent light from entering the
4. Summary of Test Method
test cell from the sides is preferred. If a viewing window is
4.1 Atotalofsixtoeighttubescontaining360mLofsample includedinthedesign,thisviewingwindowshallbefittedwith
each are heated at 120 °C with oxygen in the presence of an
a suitable opaque cover and be kept closed when no observa-
iron-copper catalyst. Each tube is removed over time and the
tion is being made.
sample is analyzed by Test Method D2272 and the insolubles
6.2.1.2 If glass heating baths are used, the bath shall be
are measured until the RPVOT residual ratio reaches below
wrapped with aluminum foil or other opaque material.
25 % or an agreed-upon percentage or specified time. Test run
6.2.1.3 Bright light entering the test cell from directly
for a specified time(s) may be run using a single tube or as
overhead can be eliminated by use of an opaque shield.
many as specified by the requestor. The mass of insoluble
6.3 Flowmeter, with a flow capacity of at least 3 L of
material of each oil sample is determined gravimetrically by
oxygen/hour, and an accuracy of 60.1 L⁄h.
filtration of a 100 g oil sample through a membrane filter with
pore size 1 µm. The insoluble mass (mg/kg oil) is plotted
6.4 Heating Bath Thermometer,ASTMSolventsDistillation
against RPVOT residual ratio. The insoluble mass in milli-
Thermometer having a range from 98 °C to 152 °C and
grams per kilogram oil at 25 % or an agreed-upon RPVOT
conforming to the requirements for Thermometer 41C as
residual ratio or specified time is reported.
prescribed in Specification E1, or for Thermometer 81C as
prescribed in Specifications for IP Standard Thermometers.
5. Significance and Use
Alternatively,temperature-measuringdevicesofequalorbetter
5.1 Insoluble material may form in oils that are subjected to
accuracy and precision may be used.
oxidizing conditions.
6.5 Oxidation Cell Thermometer, A 76 mm immersion LIG
5.2 Significant formation of oil insolubles or metal corro-
having a range of 110 °C to 130 °C, graduated in 0.1 °C, total
sion products, or both, during this test may indicate that the oil
length of 300 mm 6 5 mm, and stem diameter of 6.0 mm to
will form insolubles or corrode metals, or both, resulting in
7.0 mm.Alternatively, temperature-measuring devices or DCT,
varnish formation during field service. The level of varnish
of equal or better accuracy and precision may be used.
formation in service will be dependent on many factors
Temperature of the sample shall be measured at 76 mm from
(turbinedesign,reservoirtemperature,duty-cycle,forexample.
the top of the sample. See Fig. 2 and Fig. 3.
peaking, cycling, or base-load duty, maintenance, and so forth)
NOTE 1—Temperature gradient within the sample may exist from the
and a direct correlation between results in this test and field
heating system and temperature control design.
varnish formation are yet to be established.
6.6 Wire Coiling Mandrel, as shown in Fig. 4.
5.3 Oxidation condition at 120 °C under accelerated oxida-
6.7 Thermometer Bracket, for holding the oxidation cell
tion environment of Test Method D4310 and measurement of
thermometer, of 18-8 stainless steel, having the dimensions
sludge and RPVOTvalue could reflect a practical oil quality in
shown in Fig. 5.The thermometer is held in the bracket by two
actual turbine operations. Results from this test should be used
fluoro-elastomer O-rings of approximately 5 mm inside diam-
together with other key lubricant performance indicators (in-
eter. Alternatively, thin stainless steel wire may be used.
cluding other established oxidation and corrosion tests) to
indicate suitability for service. 6.8 Abrasive Cloth, silicon carbide, 100 grit with cloth
backing.
6. Apparatus
6.9 Flexible Tubing, poly vinyl chloride approximately
6.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,
1 3
6.4 mm( ⁄4 in.)insidediameterwitha2.4 mm( ⁄32 in.)wallfor
consisting of a test tube, condenser, and oxygen delivery tube.
delivery of oxygen to the oxidation cell.
It is recommended to have a test tube with a calibration line at
6.10 Membrane Filters, white, plain, 47 mm in diameter,
360 mL(maximum error 1 mL). This calibration applies to the
test tube without inserts at 20 °C. pore size 1 µm. The recommended membrane filters are PTFE
and cellulose acetate plus nitrocellulose material.
6.2 Heating Bath, thermostatically controlled, capable of
maintaining the oil sample in the oxidation cell at a tempera-
6.11 Filter Holder, 47 mm, consisting of a borosilicate glass
ture of 120 °C 6 0.5 °C, fitted with a suitable stirring device to
funnel and a funnel base with a coarse grade fritted-glass filter
provide a uniform temperature throughout the bath, and large
support with a length of 40 µm to 60 µm, or stainless steel
enoughtoholdthedesirednumberofoxidationcellsimmersed
screen support such that the filter can be clamped between the
in the heating bath to a depth of 355 mm 6 10 mm. Heated
ground-glass sealing surfaces of the funnel and its base by
metal block baths meeting the test method requirements may
means of a metal clamp.
also be used.
6.12 Weighing Bottle, cylindrical body with ground-glass
6.2.1 Studies have suggested that direct sunlight or artificial
stopper; approximate inside diameter 65 mm, height of body
light may adversely influence the results of this test. To
45 mm, capacity 60 mL.
minimize effects of light exposure on the lubricant being
tested, light shall be excluded from the lubricant by one or 6.13 Vacuum Source, to provide pressure reduction to
more of the following ways: 13.3 kPa 6 0.7 kPa (100 mm 6 5 mm Hg) absolute pressure.
D7873 − 13 (2017)
NOTE 1—All dimensions are in millimetres (inches).
NOTE 2—The oxidation test tube has a calibration line at 360 mL. This calibration applies to the test tube alone at 20 °C.
NOTE 3—Open tube ends to be ground and fire-polished.
FIG. 1 Oxidation Cell
D7873 − 13 (2017)
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available.
7.2 Reagent Water, Unless otherwise indicated, reference to
water shall be understood to mean distilled, deionized water as
defined by Type I or Type II in Specification D1193 or Grade
3 in ISO 3696.
7.3 Acetone, Reagent grade. (Warning—Health hazard,
flammable.)
7.4 Cleaning Reagent, cleaning by a 24 h soak at room
temperature in a free rinsing liquid acid cleaner with a pH of 2
to 4.5.
7.5 n-heptane, Reagent grade. (Warning—Flammable.
Harmful if inhaled.)
7.6 Isopropyl Alcohol, Reagent grade. (Warning—
Flammable.)
7.7 Catalyst Wires,
7.7.1 Low-Metalloid Steel Wire—1.59 mm (0.0625 in.) in
diameter (No. 16 Washburn and Moen Gage).
NOTE 2—Carbon steel wire, soft bright annealed and free from rust of
Grade 1008 as described in Specification A510M is satisfactory. Similar
wire conforming to Specification E230/E230M is also satisfactory
7.8 Electrolytic Copper Wire, 1.63 mm (0.064 in.) in diam-
eter (No. 16 Imperial Standard Wire Gage or No. 14American
Wire Gage), 99.9 % purity, conforming to Specification B1.
NOTE 3—Alternatively, suitably prepared steel and copper catalyst coils
may be purchased from a supplier.
7.9 Detergent, free rinsing, water-soluble, anionic detergent
FIG. 2 Oxidation Cell with Thermometer
with a pH of 9.5 to 11.
7.10 Oxygen—(Warning—Oxygen vigorously accelerates
combustion.) 99.5 % minimum purity, with pressure regulation
adequate to maintain a constant flow of gas through the
apparatus. The use of a two-stage pressure regulator on tank
oxygen is recommended.
8. Sampling
8.1 Samples for this test can come from tanks, drums, small
containers, or even operating equipment. Therefore, use the
applicable apparatus and techniques described in Practice
D4057.
FIG. 3 76 mm Immersion LIG Thermometer
8.2 For one single determination at a specified time the
minimum required sample size is 360 mL. However, 6 to 8
tubes will be required to develop the data points to obtain the
sludge mass at 25 % or agreed-upon residual RPVOT ratio by
6.14 Cooling Vessel, A desiccator or other type of tightly
logarithmic interpolation. Therefore, approximately 2200 mL
covered vessel for cooling the weighing vessels before weigh-
to 2900 mL will be required for this test.
ing. The use of a drying agent is not recommended.
6.15 Drying Oven, capable of maintaining a temperature of
70 °C 6 5 °C.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
6.16 Forceps, having unserrated tips.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
6.17 Rubber Policeman.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
6.18 Pipette Bulb. MD.
D7873 − 13 (2017)
FIG. 4 Mandrel for Winding Catalyst Coils
wire, 225 mm 6 5 mm (8.9 in. 6 0.2 in.) overall length and 15.9 mm to
9. Preparation of Apparatus
16.5 mm (0.625 in. to 0.650 in.) inside diameter. The turns of wire are
9.1 Cleaning Catalyst—Immediately prior to winding a
evenly spaced, and two consecutive turns of the same wire are 3.96 mm to
catalyst coil, clean a 3.00 m 6 0.01 m length of iron wire and
4.22 mm (0.156 in. to 0.166 in.) apart, center to center. The mandrel
an equal length of copper wire with wads of absorbent cotton
showninFig.4isdesignedtoproducesuchacoil.Usingthismandrel,the
ironwireiswoundonathreadof14.98 mm(0.590 in.)diameter,whilethe
wet with n-heptane and foll
...
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.
´2
Designation: D7873 − 13 D7873 − 13 (Reapproved 2017)
Standard Test Method for
Determination of Oxidation Stability and Insolubles
Formation of Inhibited Turbine Oils at 120 °C Without the
Inclusion of Water (Dry TOST Method)
This standard is issued under the fixed designation D7873; 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—Section 3 was corrected editorially in May 2014.
ε NOTE—Subsection 13.2 was corrected editorially in August 2015.
1. Scope
1.1 This test method is used to evaluate the sludging tendencies of steam and gas turbine lubricants during the oxidation process
in the presence of oxygen and metal catalyst (copper and iron) at an elevated temperature. This test method may be used to evaluate
industrial oils (for example, circulating oils and so forth).
1.2 This test method is a modification of Test Method D4310 where the sludging and corrosion tendencies of the same kinds
of oils are determined after 1000 h 1000 h at 95 °C in the presence of water. Water is omitted in this modification.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 Exception—The values in parentheses in some of the figures are provided for information only for those using old
equipment based on non-SI units.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous material that can cause central
nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution
should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet
(MSDS) for details and EPA’s website—http://www.epa.gov/mercury/faq.htm—for additional information. Users should be aware
that selling mercury and/or mercury containing products into your state or country may be prohibited by law.
1.6 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.
2. Referenced Documents
2.1 ASTM Standards:
A510M Specification for General Requirements for Wire Rods and Coarse Round Wire, Carbon Steel (Metric) (Withdrawn
2011)
B1 Specification for Hard-Drawn Copper Wire
D943 Test Method for Oxidation Characteristics of Inhibited Mineral Oils
D1193 Specification for Reagent Water
D2272 Test Method for Oxidation Stability of Steam Turbine Oils by Rotating Pressure Vessel
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4310 Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils
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
D02.09.0C on Oxidation of Turbine Oils.
Current edition approved Dec. 1, 2013Dec. 1, 2017. Published January 2014December 2017. Originally approved in 2013. Last previous edition approved in 2013 as
ε2
D7873 – 13 . DOI: 10.1520/D7873-13E02.10.1520/D7873-13R17.
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.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7873 − 13 (2017)
E1 Specification for ASTM Liquid-in-Glass Thermometers
E230E230/E230M Specification andfor Temperature-Electromotive Force (EMF)(emf) Tables for Standardized Thermocouples
2.2 Other Standards:
Specification for IP Standard Thermometers
ISO 3696 Water for Analytical Laboratory Use—Specification and Test Methods
3. Terminology
3.1 Definitions:
3.1.1 sludge, n—a precipitate or sediment from oxidized mineral oil that is insoluble in n-heptane.
4. Summary of Test Method
4.1 A total of six to eight tubes containing 360 mL of sample each are heated at 120 °C with oxygen in the presence of an
iron-copper catalyst. Each tube is removed over time and the sample is analyzed by Test Method D2272 and the insolubles are
measured until the RPVOT residual ratio reaches below 25 % or an agreed-upon percentage or specified time. Test run for a
specified time(s) may be run using a single tube or as many as specified by the requestor. The mass of insoluble material of each
oil sample is determined gravimetrically by filtration of a 100 g 100 g oil sample through a membrane filter with pore size 1 μm.
The insoluble mass (mg/kg oil) is plotted against RPVOT residual ratio. The insoluble mass in milligrams per kilogram oil at 25 %
or an agreed-upon RPVOT residual ratio or specified time is reported.
5. Significance and Use
5.1 Insoluble material may form in oils that are subjected to oxidizing conditions.
5.2 Significant formation of oil insolubles or metal corrosion products, or both, during this test may indicate that the oil will
form insolubles or corrode metals, or both, resulting in varnish formation during field service. The level of varnish formation in
service will be dependent on many factors (turbine design, reservoir temperature, duty-cycle, for example. peaking, cycling, or
base-load duty, maintenance, and so forth) and a direct correlation between results in this test and field varnish formation are yet
to be established.
5.3 Oxidation condition at 120 °C under accelerated oxidation environment of Test Method D4310 and measurement of sludge
and RPVOT value could reflect a practical oil quality in actual turbine operations. Results from this test should be used together
with other key lubricant performance indicators (including other established oxidation and corrosion tests) to indicate suitability
for service.
6. Apparatus
6.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1, consisting of a test tube, condenser, and oxygen delivery tube. It
is recommended to have a test tube with a calibration line at 360 mL 360 mL (maximum error 1 mL). 1 mL). This calibration
applies to the test tube without inserts at 20 °C.
6.2 Heating Bath, thermostatically controlled, capable of maintaining the oil sample in the oxidation cell at a temperature of
120 °C 6 0.5 °C, fitted with a suitable stirring device to provide a uniform temperature throughout the bath, and large enough to
hold the desired number of oxidation cells immersed in the heating bath to a depth of 355 mm 6 10 mm. 10 mm. Heated metal
block baths meeting the test method requirements may also be used.
6.2.1 Studies have suggested that direct sunlight or artificial light may adversely influence the results of this test. To minimize
effects of light exposure on the lubricant being tested, light shall be excluded from the lubricant by one or more of the following
ways:
6.2.1.1 Use of heated liquid baths that are designed and constructed of metal, or combinations of metals and other suitable
opaque materials, that prevent light from entering the test cell from the sides is preferred. If a viewing window is included in the
design, this viewing window shall be fitted with a suitable opaque cover and be kept closed when no observation is being made.
6.2.1.2 If glass heating baths are used, the bath shall be wrapped with aluminum foil or other opaque material.
6.2.1.3 Bright light entering the test cell from directly overhead can be eliminated by use of an opaque shield.
6.3 Flowmeter, with a flow capacity of at least 3 L 3 L of oxygen/hour, and an accuracy of 60.1 60.1 L L/h.⁄h.
6.4 Heating Bath Thermometer, ASTM Solvents Distillation Thermometer having a range from 98 °C to 152 °C and conforming
to the requirements for Thermometer 41C as prescribed in Specification E1, or for Thermometer 81C as prescribed in
Specifications for IP Standard Thermometers. Alternatively, temperature-measuring devices of equal or better accuracy and
precision may be used.
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http://www.energyinst.org.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
D7873 − 13 (2017)
NOTE 1—All dimensions are in millimetres (inches).
NOTE 2—The oxidation test tube has a calibration line at 360 mL. 360 mL. This calibration applies to the test tube alone at 20 °C.
NOTE 3—Open tube ends to be ground and fire-polished.
FIG. 1 Oxidation Cell
D7873 − 13 (2017)
6.5 Oxidation Cell Thermometer, A 76 mm 76 mm immersion LIG having a range of 110 °C to 130 °C, graduated in 0.1 °C,
total length of 300 mm 6 5 mm, 300 mm 6 5 mm, and stem diameter of 6.0 mm to 7.0 mm. 7.0 mm. Alternatively,
temperature-measuring devices or DCT, of equal or better accuracy and precision may be used. Temperature of the sample shall
be measured at 76 mm 76 mm from the top of the sample. See Fig. 2 and Fig. 3.
NOTE 1—Temperature gradient within the sample may exist from the heating system and temperature control design.
6.6 Wire Coiling Mandrel, as shown in Fig. 4.
6.7 Thermometer Bracket, for holding the oxidation cell thermometer, of 18-8 stainless steel, having the dimensions shown in
Fig. 5. The thermometer is held in the bracket by two fluoro-elastomer O-rings of approximately 5 mm inside diameter.
Alternatively, thin stainless steel wire may be used.
6.8 Abrasive Cloth, silicon carbide, 100 grit with cloth backing.
1 3
6.9 Flexible Tubing, poly vinyl chloride approximately 6.4 mm 6.4 mm ( ⁄4 in.) in.) inside diameter with a 2.4 mm ( ⁄32 in.) in.)
wall for delivery of oxygen to the oxidation cell.
6.10 Membrane Filters, white, plain, 47 mm 47 mm in diameter, pore size 1 μm. 1 μm. The recommended membrane filters are
PTFE and cellulose acetate plus nitrocellulose material.
6.11 Filter Holder, 47 mm, 47 mm, consisting of a borosilicate glass funnel and a funnel base with a coarse grade fritted-glass
filter support with a length of 40 μm to 60 μm, 60 μm, or stainless steel screen support such that the filter can be clamped between
the ground-glass sealing surfaces of the funnel and its base by means of a metal clamp.
6.12 Weighing Bottle, cylindrical body with ground-glass stopper; approximate inside diameter 65 mm, 65 mm, height of body
45 mm , capacity 60 mL.45 mm, capacity 60 mL.
6.13 Vacuum Source, to provide pressure reduction to 13.3 kPa 6 0.7 kPa 0.7 kPa (100 mm 6 5 mm 5 mm Hg) absolute
pressure.
FIG. 2 Oxidation Cell with Thermometer
D7873 − 13 (2017)
FIG. 3 76 mm Immersion LIG Thermometer
6.14 Cooling Vessel, A desiccator or other type of tightly covered vessel for cooling the weighing vessels before weighing. The
use of a drying agent is not recommended.
6.15 Drying Oven, capable of maintaining a temperature of 70 °C 6 5 °C.
6.16 Forceps, having unserrated tips.
6.17 Rubber Policeman.
6.18 Pipette Bulb.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, where
such specifications are available.
7.2 Reagent Water, Unless otherwise indicated, reference to water shall be understood to mean distilled, deionized water as
defined by Type I or Type II in Specification D1193 or Grade 3 in ISO 3696.
7.3 Acetone, Reagent grade. (Warning—Health hazard, flammable.)
7.4 Cleaning Reagent, cleaning by a 24 h 24 h soak at room temperature in a free rinsing liquid acid cleaner with a pH of 2
to 4.5.
7.5 n-heptane, Reagent grade. (Warning—Flammable. Harmful if inhaled.)
7.6 Isopropyl Alcohol, Reagent grade. (Warning—Flammable.)
7.7 Catalyst Wires,
7.7.1 Low-Metalloid Steel Wire—1.59 mm (0.0625 in.) 1.59 mm (0.0625 in.) in diameter (No. 16 Washburn and Moen Gage).
NOTE 2—Carbon steel wire, soft bright annealed and free from rust of Grade 1008 as described in Specification A510M is satisfactory. Similar wire
conforming to Specification E230E230/E230M is also satisfactory
7.8 Electrolytic Copper Wire, 1.63 mm (0.064 in.) 1.63 mm (0.064 in.) in diameter (No. 16 Imperial Standard Wire Gage or No.
14 American Wire Gage), 99.9 %99.9 % purity, conforming to Specification B1.
NOTE 3—Alternatively, suitably prepared steel and copper catalyst coils may be purchased from a supplier.
7.9 Detergent, free rinsing, water-soluble, anionic detergent with a pH of 9.5 to 11.
7.10 Oxygen—(Warning—Oxygen vigorously accelerates combustion.) 99.5 %99.5 % minimum purity, with pressure
regulation adequate to maintain a constant flow of gas through the apparatus. The use of a two-stage pressure regulator on tank
oxygen is recommended.
8. Sampling
8.1 Samples for this test can come from tanks, drums, small containers, or even operating equipment. Therefore, use the
applicable apparatus and techniques described in Practice D4057.
8.2 For one single determination at a specified time the minimum required sample size is 360 mL. 360 mL. However, 6 to 8
tubes will be required to develop the data points to obtain the sludge mass at 25 % or agreed-upon residual RPVOT ratio by
logarithmic interpolation. Therefore, approximately 2200 mL to 2900 mL 2900 mL will be required for this test.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmaco
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