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ASTM D893-05

(Test Method)

Standard Test Method for Insolubles In Used Lubricating Oils

Standard Test Method for Insolubles In Used Lubricating Oils

SCOPE
1.1 This test method covers the determination of pentane and toluene insolubles in used lubricating oils.
1.2 Procedure A covers the determination of insolubles without the use of coagulant in the pentane. It provides an indication of the materials that can readily be separated from the oil-solvent mixtures by centrifuging.
1.3 Procedure B covers the determination of insolubles in oils containing detergents and employs a coagulant for both the pentane and toluene insolubles. In addition to the materials separated by using Procedure A, this coagulation procedure separates some finely divided materials that may be suspended in the oil. Note 1
Results obtained by Procedures A and B should not be compared since they usually give different values. The same procedure should be employed when comparing values obtained periodically on an oil in use or when comparing results determined by two or more laboratories.
1.4 The values stated in acceptable SI units are to be regarded as the standard.
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. For specific precautionary statements, see , , , , and .

General Information

Status
Historical
Publication Date
31-Jan-2005
ICS
75.080 - Petroleum products in general
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.06.0B - Physical Testing
Current Stage
Ref Project

Relations

Replaces
ASTM D893-97(2002)e1 - Standard Test Method for Insolubles In Used Lubricating Oils
Effective Date
01-Feb-2005
Replaced By
ASTM D893-05a - Standard Test Method for Insolubles In Used Lubricating Oils
Effective Date
01-Nov-2005
Referred By
ASTM D5372-20 - Standard Guide for Evaluation of Hydrocarbon Heat Transfer Fluids
Effective Date
01-Feb-2005
Referred By
ASTM D7317-07(2019) - Standard Test Method for Coagulated Pentane Insolubles in Used Lubricating Oils by Paper Filtration (LMOA Method)
Effective Date
01-Feb-2005
Referred By
ASTM D5704-22a - Standard Test Method for Evaluation of the Thermal and Oxidative Stability of Lubricating Oils Used for Manual Transmissions and Final Drive Axles
Effective Date
01-Feb-2005
Referred By
ASTM D6224-22 - Standard Practice for In-Service Monitoring of Lubricating Oil for Auxiliary Power Plant Equipment
Effective Date
01-Feb-2005
Referred By
ASTM D7155-20 - Standard Practice for Evaluating Compatibility of Mixtures of Turbine Lubricating Oils
Effective Date
01-Feb-2005
Referred By
ASTM D7665-22 - Standard Guide for Evaluation of Biodegradable Heat Transfer Fluids
Effective Date
01-Feb-2005

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ASTM D893-05 - Standard Test Method for Insolubles In Used Lubricating OilsASTM D893-05 - Standard Test Method for Insolubles In Used Lubricating Oils
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ASTM D893-05 - Standard Test Method for Insolubles In Used Lubricating Oils
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation:D893–05
Standard Test Method for
1
Insolubles in Used Lubricating Oils
This standard is issued under the fixed designation D 893; 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 (ϵ) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of pentane
D 4177 Practice for Automatic Sampling of Petroleum and
and toluene insolubles in used lubricating oils.
Petroleum Products
1.2 Procedure A covers the determination of insolubles
without the use of coagulant in the pentane. It provides an
3. Terminology
indication of the materials that can readily be separated from
3.1 Definitions:
the oil-solvent mixtures by centrifuging.
3.1.1 coagulate, v—to cause to become viscous or thick-
1.3 Procedure B covers the determination of insolubles in
ened into a coherent mass.
oilscontainingdetergentsandemploysacoagulantforboththe
3.1.2 coagulated pentane insolubles, n—in used oil analy-
pentane and toluene insolubles. In addition to the materials
sis, separated matter that results when a coagulant is added to
separated by using Procedure A, this coagulation procedure
a solution of used oil in pentane.
separates some finely divided materials that may be suspended
3.1.2.1 Discussion—The addition of a coagulant will aid in
in the oil.
separating finely divided materials that may have been held in
NOTE 1—Results obtained by Procedures A and B should not be
suspension because of the dispersant characteristics of the oil.
compared since they usually give different values. The same procedure
3.1.3 coagulated toluene insolubles, n—in used oil analysis,
should be employed when comparing values obtained periodically on an
coagulated and separated matter not soluble in pentane or
oil in use or when comparing results determined by two or more
toluene.
laboratories.
3.1.4 pentane insolubles, n—in used oil analysis, separated
1.4 The values stated in acceptable SI units are to be
matter resulting when a used oil is mixed with pentane.
regarded as the standard.
3.1.4.1 Discussion—In this test method, the separation is
1.5 This standard does not purport to address all of the
effected by centrifugation.
safety concerns, if any, associated with its use. It is the
3.1.5 toluene insolubles, n—in used oil analysis, the portion
responsibility of the user of this standard to establish appro-
of pentane insolubles not soluble in toluene.
priate safety and health practices and determine the applica-
3.1.6 used oil, n—any oil that has been in a piece of
bility of regulatory limitations prior to use. For specific
equipment (for example, an engine, gearbox, transformer, or
precautionary statements, see 7.7, 7.8, 7.9, 9.1, and 9.7.
turbine), whether operated or not.
3.1.6.1 Discussion—In this test method, the oil can be any
2. Referenced Documents
oil that has been used for lubrication.
2
2.1 ASTM Standards:
3.2 Definitions of Terms Specific to This Standard:
D 1193 Specification for Reagent Water
3.2.1 insoluble resins, n—in used oil analysis, separated
matter soluble in toluene but not pentane.
3.2.1.1 Discussion—Insoluble resins can be calculated for
1
This test method is under the jurisdiction of ASTM Committee D02 on
either Procedue A or B by subtracting the toluene insolubles
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
from the pentane insolubles.
D02.06 on Analysis of Lubricants.
Current edition approved Feb. 1, 2005. Published February 2005. Originally
ϵ1
4. Summary of Test Method
approved in 1967. Last previous edition approved in 2002 as D 893 – 97 (2002) .
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 Procedure A—Arepresentative sample of used lubricat-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ing oil is mixed with pentane and centrifuged. The oil solution
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
is decanted and the precipitate washed twice with pentane,
*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

---------------------- Page: 1 ----------------------
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
D893–05
dried, and weighed to
...

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ASTM D4177-22e1(Practice)
Standard Practice for Automatic Sampling of Petroleum and Petroleum Products

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4.1 Representative samples of petroleum and petroleum products are required for the determination of chemical and physical properties, which are used to establish standard volumes, prices, and compliance with commercial terms and regulatory requirements. This practice does not cover sampling of electrical insulating oils and hydraulic fluids. This practice does not address how to sample crude at temperatures below the freezing point of water.
PART I—General
This part is applicable to all petroleum liquid sampling whether it be crude oil or refined products. Review this section before designing or installing any automatic sampling system.
SCOPE
1.1 This practice describes general procedures and equipment for automatically obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container. This practice also provides additional specific information about sample container selection, preparation, and sample handling. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3). This practice does not cover sampling of electrical insulating oils and hydraulic fluids.  
1.2 Table of Contents:    
Section  
INTRODUCTION  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Significance and Use  
4  
PART I–GENERAL  
Representative Sampling Components  
5  
Design Criteria  
6  
Automatic Sampling Systems  
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Sampling Location  
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Mixing of the Flowing Stream  
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Proportionality  
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Sample Extractor Grab Volume  
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Containers  
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Sample Handling and Mixing  
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Control Systems  
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Sample System Security  
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System Proving (Performance Acceptance Tests)  
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Performance Monitoring  
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Crude Oil  
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PART III–REFINED PRODUCTS  
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KEYWORDS  
Keywords  
20  
ANNEXES  
Calculations of the Margin of Error based on Number of Sample Grabs  
Annex A1  
Theoretical Calculations for Selecting the Sampler Probe Location  
Annex A2  
Portable Sampling Units  
Annex A3  
Profile Performance Test  
Annex A4  
Sampler Acceptance Test Data  
Annex A5  
APPENDIXES  
Design Data Sheet for Automatic Sampling System  
Appendix X1  
Comparisons of Percent Sediment and Water versus Unloading Time Period  
Appendix X2  
Sampling Frequency and Sampling System Monitoring Spreadsheet  
Appendix X3  
Sampling System Monitoring—Additional Diagnostics  
Appendix X4  
1.3 Units—The values stated in either SI units or US Customary (USC) units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard. Except where there is no direct SI equivalent, such as for National Pipe Threads/diameters, or tubing.  
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ASTM D4057-22(Practice)
Standard Practice for Manual Sampling of Petroleum and Petroleum Products

SIGNIFICANCE AND USE
4.1 Samples of petroleum and petroleum products are obtained for many reasons, including the determination of chemical and physical properties. These properties may be used for: calculating standard volumes; establishing product value; and often safety and regulatory reporting.  
4.2 There are inherent limitations when performing any type of sampling, any one of which may affect the representative nature of the sample. As examples, a spot sample provides a sample from only one particular point in the tank, vessel compartment, or pipeline. In the case of running or all-level samples, the sample only represents the column of material from which it was taken.  
4.3 Based on the product, and testing to be performed, this practice provides guidance on sampling equipment, container preparation, and manual sampling procedures for petroleum and petroleum products of a liquid, semi-liquid, or solid state, from the storage tanks, flowlines, pipelines, marine vessels, process vessels, drums, cans, tubes, bags, kettles, and open discharge streams into the primary sample container.
SCOPE
1.1 This practice covers procedures and equipment for manually obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container are described. Procedures are also included for the sampling of free water and other heavy components associated with petroleum and petroleum products.  
1.2 This practice also addresses the sampling of semi-liquid or solid-state petroleum products. For the sampling of green petroleum coke, see Practice D8145. For the sampling of calcined petroleum coke, see Practice D6970.  
1.3 This practice provides additional specific information about sample container selection, preparation, and sample handling.  
1.4 This practice does not cover sampling of electrical insulating oils and hydraulic fluids. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3).  
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1.6 Units—The values stated in SI units are to be regarded as the standard. USC units are reflected in parentheses.  
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ASTM D5291-21(Test Method)
Standard Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Petroleum Products and Lubricants

SIGNIFICANCE AND USE
5.1 This is the first ASTM standard covering the simultaneous determination of carbon, hydrogen, and nitrogen in petroleum products and lubricants.  
5.2 Carbon, hydrogen, and particularly nitrogen analyses are useful in determining the complex nature of sample types covered by this test method. The CHN results can be used to estimate the processing and refining potentials and yields in the petrochemical industry.  
5.3 The concentration of nitrogen is a measure of the presence of nitrogen containing additives. Knowledge of its concentration can be used to predict performance. Some petroleum products also contain naturally occurring nitrogen. Knowledge of hydrogen content in samples is helpful in addressing their performance characteristics. Hydrogen to carbon ratio is useful to assess the performance of upgrading processes.
SCOPE
1.1 These test methods cover the instrumental determination of carbon, hydrogen, and nitrogen in laboratory samples of petroleum products and lubricants. Values obtained represent the total carbon, the total hydrogen, and the total nitrogen.  
1.2 These test methods are applicable to samples such as crude oils, fuel oils, additives, and residues for carbon and hydrogen and nitrogen analysis. These test methods were tested in the concentration range of at least 75 % to 87 % by mass for carbon, at least 9 % to 16 % by mass for hydrogen, and  
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1.4 These test methods are not recommended for the analysis of volatile materials such as gasoline, gasoline-oxygenate blends, or gasoline type aviation turbine fuels.  
1.5 The results of these tests can be expressed as mass % carbon, hydrogen or nitrogen.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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.  
1.8 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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ASTM
ASTM D6304-20(Test Method)
Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration

SIGNIFICANCE AND USE
5.1 A knowledge of the water content is important in the manufacturing, purchase, sale, or transfer of petroleum products to help in predicting their quality and performance characteristics.  
5.2 The presence of moisture could lead to premature corrosion and wear, an increase in the debris load resulting in diminished lubrication and premature plugging of filters, an impedance in the effect of additives, and undesirable support of deleterious bacterial growth.
SCOPE
1.1 This test method covers the direct determination of entrained water in petroleum products and hydrocarbons using automated instrumentation. This test method also covers the indirect analysis of water thermally removed from samples and swept with dry inert gas into the Karl Fischer titration cell. Mercaptan, sulfide (S– or H2S), sulfur, and other compounds are known to interfere with this test method (see Section 6). The precision statement of this method covers the nominal range of 20 mg/kg to 25 000 mg/kg for Procedure A, 30 mg/kg to 2100 mg/kg for Procedure B, and 20 mg/kg to 360 mg/kg for Procedure C.  
1.2 This test method is intended for use with commercially available coulometric Karl Fischer reagents and for the determination of water in additives, lube oils, base oils, automatic transmission fluids, hydrocarbon solvents, and other petroleum products. By proper choice of the sample size, this test method may be used for the determination of water from mg/kg to percent level concentrations.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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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