Standard Test Method for Precipitation Number of Lubricating Oils

SIGNIFICANCE AND USE
4.1 Fully refined petroleum oils normally contain no naphtha insoluble material. Semirefined or black oils frequently contain some naphtha insoluble material (sometimes referred to as asphaltenes ). This test measures the amount of naphtha insoluble material in the oil. This quantity is reported as the precipitation number.
SCOPE
1.1 This test method covers the determination of the precipitation number of steam cylinder stocks and black oils, and can be used for other lubricating oils.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.  
1.4 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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D91 − 02 (Reapproved 2017)
Standard Test Method for
1,2
Precipitation Number of Lubricating Oils
This standard is issued under the fixed designation D91; 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.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope lubricating oil are mixed with 90 mL of ASTM precipitation
naphtha, and centrifuged under the conditions of the test.
1.1 This test method covers the determination of the pre-
cipitation number of steam cylinder stocks and black oils, and
4. Significance and Use
can be used for other lubricating oils.
4.1 Fully refined petroleum oils normally contain no naph-
1.2 The values stated in SI units are to be regarded as
tha insoluble material. Semirefined or black oils frequently
standard. No other units of measurement are included in this
contain some naphtha insoluble material (sometimes referred
standard.
to as asphaltenes ). This test measures the amount of naphtha
1.3 This standard does not purport to address all of the
insoluble material in the oil. This quantity is reported as the
safety concerns, if any, associated with its use. It is the
precipitation number.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use.
1.4 This international standard was developed in accor- 5.1 Centrifuge Tube, cone-shaped, conforming to the di-
dance with internationally recognized principles on standard- mensions given in Fig. 1, and made of thoroughly annealed
ization established in the Decision on Principles for the glass. The graduations, numbered as shown in Fig. 1, shall be
Development of International Standards, Guides and Recom- clearanddistinct,andthemouthshallbeconstructedinashape
mendations issued by the World Trade Organization Technical suitable for closure with a cork. Scale-error tolerances and
Barriers to Trade (TBT) Committee. smallest graduations between various calibration marks are
given in Table 1 and apply to calibrations made with air-free
2. Referenced Documents
water at 20 °C.
2.1 ASTM Standards:
5.2 Centrifuge, meeting all the safety requirements for
D4057 Practice for Manual Sampling of Petroleum and
normal use and capable of whirling two or more filled
Petroleum Products
centrifuge tubes at a speed which can be controlled to give a
D4177 Practice for Automatic Sampling of Petroleum and
relative centrifugal force (rcf) between 600 and 700 at the tips
Petroleum Products
of the tubes. The revolving head, trunnion rings, and trunnion
cups, including the rubber cushion, shall be soundly con-
3. Terminology
structed to withstand the maximum centrifugal force capable of
3.1 Definitions of Terms Specific to This Standard: being delivered by the power source. The trunnion cups and
3.1.1 ASTM precipitation number, of lubricating oils, n—the cushions shall firmly support the tubes when the centrifuge is
number of millilitres of precipitate formed when 10 mL of in motion.The centrifuge shall be enclosed by a metal shield or
case strong enough to eliminate danger if any breakage occurs.
Calculate the speed of the rotating head by means of the
This test method is under the jurisdiction of ASTM Committee D02 on
following equation:
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
speed, r/min 5 1337 =rcf/d (1)
Current edition approved July 1, 2017. Published July 2017. Originally approved
ɛ1
in 1921. Last previous edition approved in 2012 as D91 – 02 (2012) . DOI: where:
10.1520/D0091-02R17.
rcf = relative centrifugal force, and
This test method has been adopted for use by government agencies to replace
d = diameter of swing, in mm, measured between tips of
Method 3101 of Federal Test Method Standard No. 791b.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or opposite tubes when in rotating position.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Table 2 shows the relationship between diameter swing, rcf,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. and revolutions per minute.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D91 − 02 (2017)
to the 100 mL mark with hexanes and close tightly with a
softened cork (not a rubber stopper). Then invert each tube at
least 20 times, allowing the liquid to drain thoroughly
...


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: D91 − 02 (Reapproved 2012) D91 − 02 (Reapproved 2017)
Standard Test Method for
1,2
Precipitation Number of Lubricating Oils
This standard is issued under the fixed designation D91; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
ε NOTE—Subsection 5.2 was corrected editorially in July 2016.
1. Scope
1.1 This test method covers the determination of the precipitation number of steam cylinder stocks and black oils, and can be
used for other lubricating oils.
1.2 The values stated in acceptable SI units are to be regarded as the standard. No other units of measurement are included in
this standard.
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.
1.4 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:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 ASTM precipitation number, of lubricating oils, n—the number of millilitres of precipitate formed when 10 mL of
lubricating oil are mixed with 90 mL of ASTM precipitation naphtha, and centrifuged under the conditions of the test.
4. Significance and Use
4.1 Fully refined petroleum oils normally contain no naphtha insoluble material. Semirefined or black oils frequently contain
some naphtha insoluble material (sometimes referred to as asphaltenes ). This test measures the amount of naphtha insoluble
material in the oil. This quantity is reported as the precipitation number.
5. Apparatus
5.1 Centrifuge Tube, cone-shaped, conforming to the dimensions given in Fig. 1, and made of thoroughly annealed glass. The
graduations, numbered as shown in Fig. 1, shall be clear and distinct, and the mouth shall be constructed in a shape suitable for
closure with a cork. Scale-error tolerances and smallest graduations between various calibration marks are given in Table 1 and
apply to calibrations made with air-free water at 20 °C.
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 Nov. 1, 2012July 1, 2017. Published November 2012July 2017. Originally approved in 1921. Last previous edition approved in 20072012 as
ɛ1
D91 – 02 (2007).(2012) . DOI: 10.1520/D0091-02R12E01.10.1520/D0091-02R17.
This test method has been adopted for use by government agencies to replace Method 3101 of Federal Test Method Standard No. 791b.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D91 − 02 (2017)
NOTE 1—For volumetric tolerances see Table 1.
FIG. 1 ASTM Cone-Shaped Centrifuge Tube
TABLE 1 Calibration Tolerances for 200 mm Centrifuge Tube
Range, mL Subdivision, mL Volume Tolerance, mL
0 to 0.1 0.05 ±0.02
Above 0.1 to 0.3 0.05 ±0.03
Above 0.3 to 0.5 0.05 ±0.05
Above 0.5 to 1.0 0.10 ±0.05
Above 1.0 to 2.0 0.10 ±0.10
Above 2.0 to 3.0 0.20 ±0.10
Above 3.0 to 5.0 0.5 ±0.20
Above 5.0 to 10 1.0 ±0.50
Above 10 to 25 5.0 ±1.00
Above 25 to 100 25 ±1.00
5.2 Centrifuge, meeting all the safety requirements for normal use and capable of whirling two or more filled centrifuge tubes
at a speed which can be controlled to give a relative centrifugal force (rcf) between 600 and 700 at the tips of the tubes. The
revolving head, trunnion rings, and trunnion cups, including the rubber cushion, shall be soundly constructed to withstand the
maximum centrifugal force capable of being delivered by the power source. The trunnion cups and cushions shall firmly support
the tubes when the
...

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