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ASTM D974-02

(Test Method)

Standard Test Method for Acid and Base Number by Color-Indicator Titration

Standard Test Method for Acid and Base Number by Color-Indicator Titration

SCOPE
1.1 This test method covers the determination of acidic or basic constituents (Note 1) in petroleum products and lubricants soluble or nearly soluble in mixtures of toluene and isopropyl alcohol. It is applicable for the determination of acids or bases whose dissociation constants in water are larger than 109; extremely weak acids or bases whose dissociation constants are smaller than 109 do not interfere. Salts react if their hydrolysis constants are larger than 109.
Note 1—In new and used oils, the constituents considered to have acidic characteristics include organic and inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, and addition agents such as inhibitors and detergents. Similarly, constituents considered to have basic properties include organic and inorganic bases, amino compounds, salts of weak acids (soaps), basic salts of polyacidic bases, salts of heavy metals, and addition agents such as inhibitors and detergents.
Note 2—This test method is not suitable for measuring the basic constituents of many basic additive-type lubricating oils. Test Method D 4739 can be used for this purpose.
1.2 This test method can be used to indicate relative changes that occur in an oil during use under oxidizing conditions. Although the titration is made under definite equilibrium conditions, the method does not measure an absolute acidic or basic property that can be used to predict performance of an oil under service conditions. No general relationship between bearing corrosion and acid or base numbers is known.
Note 3—Oils, such as many cutting oils, rustproofing oils, and similar compounded oils, or excessively dark-colored oils, that cannot be analyzed for acid number by this test method due to obscurity of the color-indicator end point, can be analyzed by Test Method D 664. The acid numbers obtained by this color-indicator test method need not be numerically the same as those obtained by Test Method D 664, the base numbers obtained by this color indicator test method need not be numerically the same as those obtained by Test Method D 4739, but they are generally of the same order of magnitude.
1.3 The values stated in acceptable SI units are to be regarded as the 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.

General Information

Status
Historical
Publication Date
09-Jun-2002
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
D02.06.0A - Chemical Analysis
Current Stage
Ref Project

Relations

Replaces
ASTM D974-01 - Standard Test Method for Acid and Base Number by Color-Indicator Titration
Effective Date
10-Jun-2002
Replaced By
ASTM D974-02e1 - Standard Test Method for Acid and Base Number by Color-Indicator Titration
Effective Date
10-Jun-2002
Referred By
ASTM D3339-21 - Standard Test Method for Acid Number of Petroleum Products by Semi-Micro Color Indicator Titration
Effective Date
10-Jun-2002
Referred By
ASTM D5282-05(2020) - Standard Test Methods for Compatibility of Construction Material with Silicone Fluid Used for Electrical Insulation
Effective Date
10-Jun-2002
Referred By
ASTM D6224-22 - Standard Practice for In-Service Monitoring of Lubricating Oil for Auxiliary Power Plant Equipment
Effective Date
10-Jun-2002
Referred By
ASTM D664-18e2 - Standard Test Method for Acid Number of Petroleum Products by Potentiometric Titration
Effective Date
10-Jun-2002
Referred By
ASTM D7415-22 - Standard Test Method for Condition Monitoring of Sulfate By-Products in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry
Effective Date
10-Jun-2002
Referred By
ASTM D8029-18 - Standard Specification for Biodegradable, Low Aquatic Toxicity Hydraulic Fluids
Effective Date
10-Jun-2002
Referred By
ASTM D6469-20 - Standard Guide for Microbial Contamination in Fuels and Fuel Systems
Effective Date
10-Jun-2002
Referred By
ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
Effective Date
10-Jun-2002
Referred By
ASTM D4174-23 - Standard Practice for Cleaning, Flushing, and Purification of Petroleum Fluid Hydraulic Systems
Effective Date
10-Jun-2002
Referred By
ASTM D8240-22e1 - Standard Specification for Less-Flammable Synthetic Ester Liquids Used in Electrical Apparatus
Effective Date
10-Jun-2002
Referred By
ASTM D4304-22 - Standard Specification for Mineral and Synthetic Lubricating Oil Used in Steam or Gas Turbines
Effective Date
10-Jun-2002
Referred By
ASTM D7414-22 - Standard Test Method for Condition Monitoring of Oxidation in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry
Effective Date
10-Jun-2002
Referred By
ASTM D2440-13(2021) - Standard Test Method for Oxidation Stability of Mineral Insulating Oil
Effective Date
10-Jun-2002

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ASTM D974-02 - Standard Test Method for Acid and Base Number by Color-Indicator TitrationASTM D974-02 - Standard Test Method for Acid and Base Number by Color-Indicator Titration
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ASTM D974-02 - Standard Test Method for Acid and Base Number by Color-Indicator Titration
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Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation: D 974 – 02
British Standard 2634
Designation: 139/98
Standard Test Method for
1,2
Acid and Base Number by Color-Indicator Titration
This standard is issued under the fixed designation D 974; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
numbers obtained by this color-indicator test method need not be
1. Scope *
numerically the same as those obtained by Test Method D 664, the base
1.1 This test method covers the determination of acidic or
numbers obtained by this color indicator test method need not be
3
basic constituents (Note 1) in petroleum products and lubri-
numerically the same as those obtained by Test Method D 4739, but they
cants soluble or nearly soluble in mixtures of toluene and
are generally of the same order of magnitude.
isopropyl alcohol. It is applicable for the determination of acids
1.3 The values stated in acceptable SI units are to be
or bases whose dissociation constants in water are larger than
regarded as the standard.
−9
10 ; extremely weak acids or bases whose dissociation
1.4 This standard does not purport to address all of the
−9
constants are smaller than 10 do not interfere. Salts react if
safety concerns, if any, associated with its use. It is the
−9
their hydrolysis constants are larger than 10 .
responsibility of the user of this standard to establish appro-
NOTE 1—In new and used oils, the constituents considered to have priate safety and health practices and determine the applica-
acidic characteristics include organic and inorganic acids, esters, phenolic
bility of regulatory limitations prior to use.
compounds, lactones, resins, salts of heavy metals, and addition agents
such as inhibitors and detergents. Similarly, constituents considered to
2. Referenced Documents
have basic properties include organic and inorganic bases, amino com-
2.1 ASTM Standards:
pounds, salts of weak acids (soaps), basic salts of polyacidic bases, salts
D 117 Guide for Sampling, Test Methods, Specifications,
of heavy metals, and addition agents such as inhibitors and detergents.
and Guide for Electrical Insulating Oils of Petroleum
4
NOTE 2—This test method is not suitable for measuring the basic Origin
constituents of many basic additive-type lubricating oils. Test Method
D 664 Test Method for Acid Number of Petroleum Products
5
D 4739 can be used for this purpose.
by Potentiometric Titration
6
D 1193 Specification for Reagent Water
1.2 This test method can be used to indicate relative changes
that occur in an oil during use under oxidizing conditions. D 4175 Terminology Relating to Petroleum, Petroleum
7
Products, and Lubricants
Although the titration is made under definite equilibrium
conditions, the method does not measure an absolute acidic or D 4739 Test Method for Base Number Determination by
7
Potentiometric Titration
basic property that can be used to predict performance of an oil
under service conditions. No general relationship between
3. Terminology
bearing corrosion and acid or base numbers is known.
3.1 Definitions:
NOTE 3—Oils, such as many cutting oils, rustproofing oils, and similar
3.1.1 acid number, n—the quantity of base, expressed in
compounded oils, or excessively dark-colored oils, that cannot be ana-
milligrams of potassium hydroxide per gram of sample that is
lyzed for acid number by this test method due to obscurity of the
required to titrate a sample to a specified end point.
color-indicator end point, can be analyzed by Test Method D 664. The acid
3.1.1.1 Discussion—In this test method, the indicator is
p-naptholbenzein titrated to a green/green-brown end point in
1
This test method is under the jurisdiction of ASTM Committee D02 on
a toluene-water-isopropanol solvent.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
3.1.2 base number, n—the quantity of acid, expressed in
D02.06 on Analysis of Lubricants.
milligrams of potassium hydroxide per gram of sample that is
In the IP, this test method is under the jurisdiction of the Standardization
Committee. This test method was adopted as a joint ASTM-IP standard in 1965.
required to titrate a sample to a specified end point.
Current edition approved June 10, 2002. Published August 2002. Originally
published as D 974–48T. Last previous edition D 974–01.
2 4
This test method has been adopted for use by government agencies to replace Annual Book of ASTM Standards, Vol 10.03.
5
Method 5105 of Federal Test Method Standard No. 791b. Annual Book of ASTM Standards,
...

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SIGNIFICANCE AND USE
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1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
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5.1 New and used petroleum products can contain basic or acidic constituents that are present as additives or as degradation products formed during service, such as oxidation products. The relative amount of these materials can be determined by titrating with acids or bases. This number, whether expressed as acid number or base number, is a measure of this amount of acidic or basic substances, respectively, in the oil—always under the conditions of the test. This number is used as a guide in the quality control of lubricating oil formulations. It is also sometimes used as a measure of lubricant degradation in service; however, any condemning limits must be empirically established.  
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1.1 This test method covers the determination of acidic or basic constituents (Note 1) in petroleum products3 and lubricants soluble or nearly soluble in mixtures of toluene and isopropyl alcohol. It is applicable for the determination of acids or bases whose dissociation constants in water are larger than 10−9; extremely weak acids or bases whose dissociation constants are smaller than 10−9 do not interfere. Salts react if their hydrolysis constants are larger than 10−9.
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5.1 The results obtained by this test are a useful guideline in determining the ability of water-miscible metalworking fluids to prevent or minimize rust under specific conditions. There is usually a relationship between the results of this test and a similar ability of the subject coolant to prevent rust on nested parts or in drilled holes containing chips, etc. It must be understood, however, that conditions, metal types, etc. found in practice will not correlate quantitatively with these controlled laboratory conditions. The procedure may not be able to differentiate between two products with poor rust control due to the wide spacing between test dilutions.
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ASTM D4177-22e1(Practice)
Standard Practice for Automatic Sampling of Petroleum and Petroleum Products

SIGNIFICANCE AND USE
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  
7  
Sampling Location  
8  
Mixing of the Flowing Stream  
9  
Proportionality  
10  
Sample Extractor Grab Volume  
11  
Containers  
12  
Sample Handling and Mixing  
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Control Systems  
14  
Sample System Security  
15  
System Proving (Performance Acceptance Tests)  
16  
Performance Monitoring  
17  
PART II–CRUDE OIL  
Crude Oil  
18  
PART III–REFINED PRODUCTS  
Refined Products  
19  
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.  
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.  
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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).  
1.5 The procedures described in this practice may also be applicable in sampling most non-corrosive liquid industrial chemicals provided that all safety precautions specific to these chemicals are followed. Also, refer to Practice E300. The procedures described in this practice are also applicable to sampling liquefied petroleum gases and chemicals. Also refer to Practices D1265 and D3700. The procedure for sampling bituminous materials is described in Practice D140. Practice D4306 provides guidance on sample containers and preparation for sampling aviation fuel.  
1.6 Units—The values stated in SI units are to be regarded as the standard. USC units are reflected in parentheses.  
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 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  
1.3 The nitrogen test method is not applicable to light materials or those containing  
1.3.1 However, using Test Method D levels of 0.1 % by mass nitrogen in lubricants could be determined.  
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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