D02.06 - Analysis of Liquid Fuels and Lubricants

SIGNIFICANCE AND USE
5.1 The carbon residue value of burner fuel serves as a rough approximation of the tendency of the fuel to form deposits in vaporizing pot-type and sleeve-type burners. Similarly, provided alkyl nitrates are absent (or if present, provided the test is performed on the base fuel without additive) the carbon residue of diesel fuel correlates approximately with combustion chamber deposits.  
5.2 The carbon residue value of motor oil, while at one time regarded as indicative of the amount of carbonaceous deposits a motor oil would form in the combustion chamber of an engine, is now considered to be of doubtful significance due to the presence of additives in many oils. For example, an ash-forming detergent additive may increase the carbon residue value of an oil yet will generally reduce its tendency to form deposits.  
5.3 The carbon residue value of gas oil is useful as a guide in the manufacture of gas from gas oil, while carbon residue values of crude oil residuums, cylinder and bright stocks, are useful in the manufacture of lubricants.
SCOPE
1.1 This test method covers the determination of the amount of carbon residue (Note 1) left after evaporation and pyrolysis of an oil, and is intended to provide some indication of relative coke-forming propensities. This test method is generally applicable to relatively nonvolatile petroleum products which partially decompose on distillation at atmospheric pressure. Petroleum products containing ash-forming constituents as determined by Test Method D482 or IP Method 4 will have an erroneously high carbon residue, depending upon the amount of ash formed (Note 2 and Note 4).  
Note 1: The term carbon residue is used throughout this test method to designate the carbonaceous residue formed after evaporation and pyrolysis of a petroleum product under the conditions specified in this test method. The residue is not composed entirely of carbon, but is a coke which can be further changed by pyrolysis. The term carbon residue is continued in this test method only in deference to its wide common usage.
Note 2: Values obtained by this test method are not numerically the same as those obtained by Test Method D524. Approximate correlations have been derived (see Fig. X1.1), but need not apply to all materials which can be tested because the carbon residue test is applied to a wide variety of petroleum products.
Note 3: The test results are equivalent to Test Method D4530, (see Fig. X1.2).
Note 4: In diesel fuel, the presence of alkyl nitrates such as amyl nitrate, hexyl nitrate, or octyl nitrate causes a higher residue value than observed in untreated fuel, which can lead to erroneous conclusions as to the coke forming propensity of the fuel. The presence of alkyl nitrate in the fuel can be detected by Test Method D4046.  
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 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.  
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 Prin...

SIGNIFICANCE AND USE
5.1 Some acids can be present in aviation turbine fuels due either to the acid treatment during the refining process or to naturally occurring organic acids. Significant acid contamination is not likely to be present because of the many check tests made during the various stages of refining. However, trace amounts of acid can be present and are undesirable because of the consequent tendencies of the fuel to corrode metals that it contacts or to impair the water separation characteristics of the aviation turbine fuel.  
5.2 This test method is designed to measure the levels of acidity that can be present in aviation turbine fuel and is not suitable for determining significant acid contamination.
SCOPE
1.1 This test method covers the determination of the acidity in aviation turbine fuel in the range from 0.000 mg/g to 0.100 mg/g KOH.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 The bromine number is useful as a measure of aliphatic unsaturation in petroleum samples. When used in conjunction with the calculation procedure described in Annex A2, it can be used to estimate the percentage of olefins in petroleum distillates boiling up to approximately 315 °C (600 °F).  
5.2 The bromine number of commercial aliphatic monoolefins provides supporting evidence of their purity and identity.
SCOPE
1.1 This test method3 covers the determination of the bromine number of the following materials:  
1.1.1 Petroleum distillates that are substantially free of material lighter than isobutane and that have 90 % distillation points (by Test Method D86) under 327 °C (626 °F). This test method is generally applicable to gasoline (including leaded, unleaded, and oxygenated fuels), kerosine, and distillates in the gas oil range that fall in the following limits:    
90 % Distillation Point, °C (°F)  
Bromine Number, max3    
Under 205 (400)  
175    
205 to 327 (400 to 626)  
10  
1.1.2 Commercial olefins that are essentially mixtures of aliphatic mono-olefins and that fall within the range of 95 to 165 bromine number (see Note 1). This test method has been found suitable for such materials as commercial propylene trimer and tetramer, butene dimer, and mixed nonenes, octenes, and heptenes. This test method is not satisfactory for normal alpha-olefins.  
Note 1: These limits are imposed since the precision of this test method has been determined only up to or within the range of these bromine numbers.  
1.2 The magnitude of the bromine number is an indication of the quantity of bromine-reactive constituents, not an identification of constituents; therefore, its application as a measure of olefinic unsaturation should not be undertaken without the study given in Annex A1.  
1.3 For petroleum hydrocarbon mixtures of bromine number less than 1.0, a more precise measure for bromine-reactive constituents can be obtained by using Test Method D2710. If the bromine number is less than 0.5, then Test Method D2710 or the comparable bromine index methods for industrial aromatic hydrocarbons, Test Methods D1492 or D5776 must be used in accordance with their respective scopes. The practice of using a factor of 1000 to convert bromine number to bromine index is not applicable for these lower values of bromine number.  
1.4 The values stated in SI units are to be regarded as the standard.  
1.4.1 Exception—The values given in parentheses are for information only.  
1.5 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. For specific warning statements, see Sections 7, 8, and 9.  
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.

SIGNIFICANCE AND USE
5.1 The tendency of oils to foam can be a serious problem in systems such as high-speed gearing, high-volume pumping, and splash lubrication. Inadequate lubrication, cavitation, and overflow loss of lubricant can lead to mechanical failure. This test method is used in the evaluation of oils for such operating conditions.
SCOPE
1.1 This test method covers the determination of the foaming characteristics of lubricating oils at 24 °C and 93.5 °C. Means of empirically rating the foaming tendency and the stability of the foam are described.  
1.2 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.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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. For specific warning statements, see Sections 7, 8, and 9.1.1.  
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.

SIGNIFICANCE AND USE
5.1 Some petroleum products are treated with mineral acid as part of the refining procedure. Obviously, any residual mineral acid in a petroleum product is undesirable. The absence of a positive indication in the test for acidity of the distillation residue or aqueous extract of a hydrocarbon liquid is an assurance of the care used in refining the fuel or solvent.
SCOPE
1.1 This test method covers the qualitative determination of the acidity of hydrocarbon liquids and their distillation residues. (Warning—Many hydrocarbon liquids are extremely flammable. Harmful if inhaled. Hydrocarbon liquid vapors can cause a flash fire.)  
1.2 If desired to determine the basicity of a hydrocarbon liquid, proceed in accordance with 9.2 or 9.3, but substitute 3 drops of phenolphthalein indicator solution for the methyl orange indicator. A pink or red color in the aqueous solution when phenolphthalein is used indicates basicity.  
1.3 The results obtained by this test method are qualitative expressions. However, for the preparation of reagents and in the procedure, acceptable SI units are to be regarded as the standard.  
1.4 This standard does not purport to address all of the safety problems, 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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products can contain basic constituents that are present as additives. The relative amount of these materials can be determined by titration with acids. The base number is a measure of the amount of basic substances in the oil always under the conditions of the test. It is sometimes used as a measure of lubricant degradation in service. However, any condemning limit shall be empirically established.  
5.2 As stated in 1.2, this test method uses a weaker acid to titrate the base than Test Method D2896, and the titration solvents are also different. Test Method D2896 uses a stronger acid and a more polar solvent system than Test Method D4739. As a result, Test Method D2896 will titrate salts of weak acids (soaps), basic salts of polyacidic bases, and weak alkaline salts of some metals. They do not protect the oil from acidic components due to the degradation of the oil. This test method may produce a falsely exaggerated base number. Test Method D4739 will probably not titrate these weak bases but, if so, will titrate them to a lesser degree of completion. It measures only the basic components of the additive package that neutralizes acids. On the other hand, if the additive package contains weak basic components that do not play a role in neutralizing the acidic components of the degrading oil, then the Test Method D4739 result may be falsely understated.  
5.3 Particular care is required in the interpretation of the base number of new and used lubricants.  
5.3.1 When the base number of the new oil is required as an expression of its manufactured quality, Test Method D2896 is preferred, since it is known to titrate weak bases that this test method may or may not titrate reliably.  
5.3.2 When the base number of in-service or at-term oil is required, this test method is preferred because in many cases, especially for internal combustion engine oils, weakly basic degradation products are possible. Test Method D2896 will titrate these, thu...
SCOPE
1.1 This test method covers a procedure for the determination of basic constituents in petroleum products and new and used lubricants. This test method resolves these constituents into groups having weak-base and strong-base ionization properties, provided the dissociation constants of the more strongly basic compounds are at least 1000 times than that of the next weaker groups. This test method covers base numbers up to 250.  
1.2 In new and used lubricants, the constituents that can be considered to have basic properties are primarily organic and inorganic bases, including amino compounds. This test method uses hydrochloric acid as the titrant, whereas Test Method D2896 uses perchloric acid as the titrant. This test method may or may not titrate these weak bases and, if so, it will titrate them to a lesser degree of completion; some additives such as inhibitors or detergents may show basic characteristics.  
1.3 When testing used engine lubricants, it should be recognized that certain weak bases are the result of the service rather than having been built into the oil. This test method can be used to indicate relative changes that occur in oil during use under oxidizing or other service conditions regardless of the color or other properties of the resulting oil. The values obtained, however, are intended to be compared with the other values obtained by this test method only; base numbers obtained by this test method are not intended to be equal to values by other test methods. Although the analysis is made under closely specified conditions, this test method is not intended to, and does not, result in reported basic properties that can be used under all service conditions to predict performance of an oil; for example, no overall relationship is known between bearing corrosion or the control of corrosive wear in the engine and base number.  
1.4 This test method was developed as an alternative for the former base numb...

SIGNIFICANCE AND USE
5.1 The tendency of oils to foam at high temperature can be a serious problem in systems such as high-speed gearing, high volume pumping, and splash lubrication. Foaming can cause inadequate lubrication, cavitation, and loss of lubricant due to overflow, and these events can lead to mechanical failure.  
5.2 Correlation between the amount of foam created or the time for foam to collapse, or both, and actual lubrication failure has not been established. Such relations should be empirically determined for foam sensitive applications.
SCOPE
1.1 This test method covers the procedure for determining the foaming characteristics of lubricating oils (specifically transmission fluid and motor oil) at 150 °C.  
1.2 Foaming characteristics of lubricating oils at temperatures up to 93.5 °C are determined by Test Method D892 or IP 146.  
1.3 The values stated in SI units are to be regarded as standard.  
1.3.1 Exception—The values given in parentheses are provided for information only.  
1.4 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.  
1.5 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.  
1.6 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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products can contain basic constituents that are present as additives or as degradation products formed during service. The amount of these additives in an oil can be determined by titrating against an acid. The base number is a measure of the amount of basic substance in the oil, always under the conditions of the test. A decrease in base number is often used as a measure of lubricant degradation, but any condemning limits must be empirically established.  
5.2 This test method uses reagents that are considered less hazardous than most reagents used in alternate base number methods. It uses pre-packaged reagents to facilitate base number determinations in the field where scientific equipment is unavailable and quick results are at a premium.
Note 1: Results obtained by this test method3 are similar to those obtained by Test Method D2896.
SCOPE
1.1 This test method covers a procedure for determining the basic constituents in petroleum products in the field or laboratory using a pre-packaged test kit. The test uses a micro-titration resulting in a visual endpoint facilitated by a color indicator.  
1.1.1 This test method covers base numbers from 0 to 20. It can be extended to higher ranges by diluting the sample or by using a smaller sample size; however, the precision data were obtained for base numbers up to 20.  
1.2 This test method can be used to indicate relative changes that occur in an oil during use under oxidizing conditions. Although the test is performed under closely specified conditions with standardized reagents, the test method does not measure an absolute basic property that can be used to predict performance of an oil under service conditions. No general relationship between bearing corrosion and base number is known.  
1.3 The values stated in SI units are to be regarded as the standard.  
1.3.1 Exception—The values given in parentheses are for information only.  
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.

SIGNIFICANCE AND USE
5.1 This test method provides a semiquantitative estimate of the acid number of lubricating oils obtained from laboratory oxidation tests using smaller amounts of sample than Test Methods D974, D664, or D3339. It has specific application in Test Method D943 and in Test Method D4871. This test method, therefore, provides a means of monitoring the relative oxidation of lubricating oils by measuring changes in acid number, at different time intervals and under various oxidizing test conditions.  
5.2 Since this test method is semiquantitative, each laboratory shall develop its own criteria for each oxidation test method for determining when to switch from this semiquantitative test method to a more precise test method for acid number.
SCOPE
1.1 This test method is a semiquantitative micro method intended for monitoring the changes in acidic constituents occurring in lubricating oils during oxidation testing, when the acid number of such oils falls within the range from 0.02 mg to 1.0 mg of potassium hydroxide per gram of sample. It is applicable to such oils as turbine oils, hydraulic oils, and other circulating oils.  
Note 1: This test method is a micro version of Test Method D974 and it produces results similar to that method.  
1.2 This test method is designed for use where sample size is limited. It shall not be used as a replacement for higher precision methods such as Test Methods D974 or D664. It shall not be used to monitor oils in-service.  
1.3 The values stated in SI units are to be regarded as the standard.  
1.3.1 Exception—The values given in parentheses are for information only.  
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.

SIGNIFICANCE AND USE
5.1 Crude oils and oil sands bitumen contain naturally occurring acidic species. Acidity of crude oil has been implicated in corrosion of distribution and process systems. The relative amount of these materials can be determined by titrating with bases. The acid number is a measure of this amount of acidic substance in the oil under the conditions of the test.  
5.2 Acid number of crude and distilled petroleum fractions has been measured by Test Method D664. Test Method D664 was developed for the analysis of lubricants and biodiesel. The titration solvent used in Test Method D664 does not properly address dissolving difficult samples such as crude oil, bitumen, and high wax samples addressed in this test method. Refer to Appendix X1.  
5.3 Test Method D974 is also not applicable to measuring acidity of crudes and highly colored samples because the indicator is not visible or it is difficult to discern a color change to detect the end point of the titration.
SCOPE
1.1 This test method covers the determination of acidic components in crude oil and petroleum products including waxes, bitumen, base stocks, and asphalts that are soluble in mixtures of xylenes and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. The values obtained by this test method may not be numerically equivalent to other acid value measurements. The range of KOH acid numbers included in the precision statement is 0.1 mg/g to 16 mg/g.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Some specific hazards statements are given in Section 7 on Safety Precautions.  
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.

SIGNIFICANCE AND USE
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.  
5.2 Since a variety of oxidation products contribute to the acid number and the organic acids vary widely in corrosive properties, the test cannot be used to predict corrosiveness of an oil under service conditions. No general correlation is known between acid number and the corrosive tendency of oils toward metals. Compounded engine oils can and usually do have both acid and base numbers in this test method.
SCOPE
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.
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 D4739 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 D664. The acid numbers obtained by this color-indicator test method need not be numerically the same as those obtained by Test Method D664, the base numbers obtained by this color indicator test method need not be numerically the same as those obtained by Test Method D4739, but they are generally of the same order of magnitude.  
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...

SIGNIFICANCE AND USE
5.1 This test method measures acidity in ethanol or ethanol blends quantitatively. Denatured fuel ethanol may contain additives such as corrosion inhibitors and detergents as well as contaminants from manufacturing that can affect the acidity of finished ethanol fuel. Very dilute aqueous solutions of low molecular mass organic acids, such as acetic acid, are highly corrosive to many metals. It is important to keep such acids at a very low level.  
5.2 Acceptable levels of acidity in ethanol or ethanol blends can vary with different specifications but in general it is below 200 mg/kg (ppm). Knowledge of the acidity can be required to establish whether the product quality meets specification.
SCOPE
1.1 This test method covers the determination of acidity as acetic acid (see Specification D4806) in commonly available grades of denatured ethanol, and ethanol blends with gasoline ranging from E95 to E30. This test method is used for determining low levels of acidity, below 200 mg/kg (ppm mass), with the exclusion of carbon dioxide.  
1.1.1 Procedure A—Developed specifically for measurement of acidity by potentiometric titration. This is the referee method.  
1.1.2 Procedure B—Developed specifically for measurement of acidity by color end point titration.  
1.2 The ethanol and ethanol blends may be analyzed directly by this test method without any sample preparation.  
1.3 Review the current and appropriate Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid procedures, and safety precautions and proper personal protective equipments.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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. Some specific hazards statements are given in Section 7 on Hazards.  
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.

SIGNIFICANCE AND USE
5.1 Lubricants can contain basic constituents that are present as additives. The relative amount of these materials can be determined by titration with acids. The base number is a measurement of the amount of basic substances in the oil under the conditions of the testing procedure.  
5.2 A primary objective of a marine cylinder lubricant is the neutralization of sulfuric acid, produced during fuel combustion, to protect the engine from corrosion. The EBas method characterizes the more efficient basic species of the lubricant reacting with acids from the beginning of the neutralization (when the lubricant milieu is basic) until an equilibrium state where the lubricant becomes slightly acidic. The use of hydrochloric acid (HCl) allows differentiating basicities of various strengths during titration.  
5.3 In marine lubricants, the constituents that can be considered to have basic properties are primarily organic and inorganic bases coming from the detergent. Basicity can also be brought to the lubricant by other components including dispersants, amino compounds, or any organic basic components. This test method uses the same titration system as that of Test Method D4739, however the evaluation and interpretation of the titration result is different. The hydrochloric acid is used as the titrant in this test method and Test Method D4739, whereas Test Method D2896 uses a stronger acid, perchloric acid. While all three methods can be considered as complementary to evaluate the basicity of lubricants, this test method is only used for marine cylinder lubricants.  
5.4 This test method measures only the efficient basicity of the lubricant, which represents only the part of the total basicity, until the point of which the lubricant becomes slightly acidic. It will depend on the components of the formulation itself. In that respect, the EBas cannot be compared to base number given by Test Methods D4739 or D2896. The EBas is then complementary information to the base numbe...
SCOPE
1.1 This test method covers a procedure for the determination of the efficient basicity (EBas) in new marine cylinder lubricants that lubricate the upper part, that is, piston-ring-cylinder area, of two-stroke marine engines.  
1.2 This test method has been developed for marine cylinder lubricants, having base number (BN) (measured by Test Method D2896) from 20 mg KOH/g to 100 mg KOH/g, and an EBas from 10 mg KOH/g to 36 mg KOH/g.  
1.3 In this test method, only the efficient basicity is determined, corresponding to the components or part of components that have a major role in neutralization of the acidic species formed in the combustion of the fuel in the marine engine. It differentiates between the fastest reacting species and the last one to react like overbasing compounds in detergent (classically mineral calcium carbonate, CaCO3). The values obtained, however, are intended to be compared with the other values obtained by this test method only; base numbers obtained by this test method are not intended to be equal to values by other test methods.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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. Some specific hazards statements are given in Sections 6 and 7.  
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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products can contain basic constituents that are present as additives. The relative amounts of these materials can be determined by titration with acids. The base number is a measure of the amount of basic substance in the oil, always under the conditions of the test. It is sometimes used as a measure of lubricant degradation in service; however, any condemning limits must be empirically established.
SCOPE
1.1 This test method covers the determination of basic constituents in petroleum products by titration with perchloric acid in glacial acetic acid.  
1.2 Procedures A and B use different titration solvent volumes and sample weights.  
Note 1: A round robin on a series of new and used oils and additive concentrates has shown that the two procedures give statistically equivalent results.  
1.3 Appendix X2 provides the use of an alternative solvent system which eliminates the use of chlorobenzene in this test method. The use of the alternative solvent gives statistically equivalent results; however, the precision is worse. Paragraph X2.5.5 provides guidance when comparing results using the two different solvents.  
1.4 The constituents that may be considered to have basic characteristics include organic and inorganic bases, amino compounds, salts of weak acids (soaps), basic salts of polyacidic bases, and salts of heavy metals.  
Note 2: This test method is applicable to both fresh oils and used oils as described in Sections 16, 17, and 19 and Appendix X1.  
1.5 This test method can be used to determine base number >300 mg KOH/g. However, the precision statement in Section 19 has been obtained only on base number ≤300 mg KOH/g.  
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. For specific warning statements, see Section 7, Section 10, and X2.2.  
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.

SIGNIFICANCE AND USE
5.1 This test method measures the acid number of oils obtained from laboratory oxidation tests using smaller amounts of sample than Test Methods D974 or D664. It has specific application in Test Method D943 in which small aliquots of oil are periodically removed for testing by Test Method D3339. This test method, therefore, provides a means of monitoring the relative oxidation of oils, by measuring changes in acid number, at different time intervals and under the various oxidizing test conditions.
SCOPE
1.1 This test method covers the determination of acidic constituents in new or used petroleum products and lubricants soluble or nearly soluble in mixtures of toluene, and isopropyl alcohol. The test method is especially intended for cases in which the amount of sample available to be analyzed is too small to allow accurate analysis by Test Methods D974 or D664. It is applicable for the determination of acids having dissociation constants in water larger than 10−9. Extremely weak acids having dissociation constants smaller than 10−9 do not interfere. Salts titrate if their hydrolysis constants are larger than 10−9.  
1.2 This test method can be used to indicate relative changes in acid number 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 property that can be used to predict performance of an oil under service conditions. No general relationship between bearing corrosion and acid number is known.  
1.3 Since this test method requires substantially less sample than Test Methods D974 or D664, it provides an advantageous means of monitoring an oxidation test by changes in acid number by (1) minimizing test sample depletion for acid number analyses and thus minimizing the disturbance of the test or (2) allowing additional acid number analyses to be made while maintaining the same test sample depletion and thus providing additional data.  
Note 1: Some oils, such as many cutting oils, rust-proofing oils, and similar compounded oils, or excessively dark-colored oils, may be more difficult to analyze by this test method due to obscurity of the color-indicator end point. These oils can be analyzed by Test Method D664 provided sufficient sample is available. However, this situation is much less likely using Test Method D3339 than using Test Method D974 due to the use of a more highly dilute sample during the titration and due to the greater stability of the end point color change. The acid numbers obtained by Test Method D3339 may or may not be numerically the same as those obtained by Test Method D664 but they should be of the same order of magnitude.
Note 2: The results obtained using this method have been found to be numerically the same as those obtained using Test Method D974, within the precision of the two methods, for new or oxidized lubricants of the type primarily intended for hydraulic or steam turbine type service. The oxidized lubricants were obtained using the Test Method D943 oxidation test. This correlation is shown by the correlation coefficient r = 0.989 with slope s = + 1.017 and intercept  y = + 0.029, calculated using the acid numbers obtained using both titration methods for the samples used for the precision statement (12.2).2  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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. For specific warning statements, see Sections 7 and 9, A1.1.4, A2.3.1, and A2.10.1.  
1.6 This international standard was developed in accordance with internationally recognized principles on sta...

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 The apparatuses used in Procedure C (see Annex A2) and Procedure D, also permit 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 four procedures for determining the evaporation loss of lubricating oils (particularly engine oils). The evaporation measured is reported as percent total loss. The test method relates to one set of operating conditions but may be readily adapted to other conditions as required.  
1.2 Procedure B and Procedure D that are in the main section of the test method provide equivalent results. Procedures A and C, which are in Annex A1 and Annex A2, have equivalent results. It has been determined that Procedures A and C show a slight bias when compared to Procedures B and D. Procedures B and D give slightly higher results versus Procedures A and C on formulated engine oils, while Procedures B and D give lower results versus Procedures A and C on basestocks. Thus, a correction factor is utilized to convert between the two sets of Procedures based on the fluid type.  
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.

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.

SIGNIFICANCE AND USE
5.1 This test method provides a measure of trace amounts of unsaturated hydrocarbons in petroleum distillates boiling up to 288 °C (550 °F). An estimate of the quantity of these materials is useful in assessing the suitability of the lighter fractions for use as reaction solvents.
SCOPE
1.1 This test method covers the determination of the amount of bromine-reactive material in petroleum hydrocarbons and is thus a measure of trace amounts of unsaturates in these materials. It is applicable to materials having bromine indexes below 1000.  
1.2 This test method is applicable only to essentially olefin-free hydrocarbons or mixtures that are substantially free from material lighter than isobutane and have a distillation end point under 288 °C (550 °F).
Note 1: This procedure has been cooperatively tested on materials with bromine indexes in the range from 100 to 1000. These materials include petroleum distillates such as straight-run and hydrocracked naphtha, reformer feed, kerosine, and aviation turbine fuel.
Note 2: Materials with bromine index greater than 1000 should be tested for bromine number using Test Method D1159/IP 130.
Note 3: Bromine index of industrial aromatic hydrocarbons should be determined using Test Method D1492 or D5776. The subcommittee is currently examining ways to achieve more consistent end point values.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.

SIGNIFICANCE AND USE
5.1 The carbon residue value of the various petroleum materials serves as an approximation of the tendency of the material to form carbonaceous type deposits under degradation conditions similar to those used in the test method, and can be useful as a guide in manufacture of certain stocks. However, care needs to be exercised in interpreting the results.  
5.2 This test method offers advantages of better control of test conditions, smaller samples, and less operator attention compared to Test Method D189, to which it is equivalent.  
5.3 Up to twelve samples may be run simultaneously, including a control sample when the vial holder shown in Fig. 1 is used exclusively for sample analysis.
FIG. 1 Sample Vial Holder and Vial
SCOPE
1.1 This test method covers the determination of the amount of carbon residue (see Note 1) formed after evaporation and pyrolysis of petroleum materials under certain conditions and is intended to provide some indication of the relative coke forming tendency of such materials.  
1.2 The test results are equivalent to the Conradson Carbon Residue test (see Test Method D189).  
Note 1: This procedure is a modification of the original method and apparatus for carbon residue of petroleum materials, where it has been demonstrated that thermogravimetry is another applicable technique.2 However, it is the responsibility of the operator to establish operating conditions to obtain equivalent results when using thermogravimetry.  
1.3 This test method is applicable to petroleum products that partially decompose on distillation at atmospheric pressure and was tested for carbon residue values of 0.10 % to 30 % (m/m). Samples expected to be below 0.10 weight % (m/m) residue should be distilled to remove 90 % (V/V) of the flask charge (see Section 9). The 10 % bottoms remaining is then tested for carbon residue by this test method.  
1.4 Ash-forming constituents, as defined by Test Method D482, or non-volatile additives present in the sample will add to the carbon residue value and be included as part of the total carbon residue value reported.  
1.5 Also in diesel fuel, the presence of alkyl nitrates, such as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon residue value than observed in untreated fuel, which may lead to erroneous conclusions as to the coke-forming propensity of the fuel. The presence of alkyl nitrate in the fuel may be detected by Test Method D4046.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 Exception—6.4 and 6.5 include inch-pound units.  
1.7 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.  
1.8 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 to determine the applicability of regulatory limitations prior to use. For specific warning statements, see 8.2.3 and 8.4.  
1.9 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.

SIGNIFICANCE AND USE
5.1 Leakage of glycol-base antifreeze into the crankcase is serious because the coolant tends to interfere with the lubricant and its ability to lubricate; it also promotes sludging. Ethylene glycol present in the coolant can increase varnish deposit formation in the crankcase as a result of glycol oxidation and the interaction between glycol and lubricant. Furthermore, because glycol is a higher boiling material than water, it will tend to stay longer in the crankcase oil than water. Lubricant displacement, sludging, and deposit formation all lead to engine malfunction and possible seizure.  
5.2 These tests are designed to detect glycol-base coolant contamination even at low levels because early detection enables corrective measures to be taken to prevent leaking coolant from accumulating and seriously damaging the engine.  
5.3 These test methods are also significant because the reagents can be packaged as a field kit, and the procedure can be followed at the site where there is a concern.
SCOPE
1.1 These test methods cover the qualitative determination of glycol-base antifreeze in used lubricating oils (mineral base) by two procedures, one using reagents in tablet form and the other using laboratory shelf reagents. Principally the test methods detect ethylene glycol but will also detect other 1,2-glycols that may be present.  
1.1.1 When a positive result is obtained and a sample of the unused oil is available, the unused oil is also tested and used as a reference.
Note 1: Since the inception of this test method (1971), there have been many changes in base stock technology and additive technology. Therefore, when available, the new, unused oil, or a sample of the same used oil, known to not contain antifreeze, is tested as a reference.  
1.2 The tablet procedure (Procedure A) is sensitive to about 100 mg/kg and the shelf reagent procedure (Procedure B) to about 300 mg/kg of ethylene glycol.  
1.3 Glycol-based coolant leaks into crankcases may not be detected or may result in a low bias using these test methods if the glycol has degraded or been thermally or otherwise oxidized. The conditions in crankcases may be such that contaminant glycols are oxidized or degraded to a degree to which the color indicator reaction does not occur or is biased enough so as to not trigger the color change. Other test methods for the detection of coolants or coolant additives in lubricating oils should be used if the results from these test methods alone are inconclusive or questionable.  
1.4 Carbohydrates such as sugars and sugar-containing substances are sometimes used for sabotage purposes. If the presence of these substances is suspected, Procedure A contains a modification to remove these interferences.  
1.5 Both procedures are adaptable to field kit use, and brief descriptions for converting to field kit form are given in Annex A1.  
1.5.1 Commercial field testing kits are available.2,3  
1.6 The results obtained by this method are qualitative expressions. However, for the preparation of reagents and in the procedures, acceptable SI units are to be regarded as the 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.

SIGNIFICANCE AND USE
5.1 This test method is a safe and fast alternative for determination of the Noack evaporation loss of a lubricant.  
5.2 The evaporation loss of a lubricant is important in the hot zones of equipment where evaporation of part of the lubricant may increase lubricant consumption.  
5.3 Some lubricant specifications cite a maximum allowable evaporative loss.
SCOPE
1.1 This test method covers the procedure for determining the Noack evaporation loss of lubricating oils using a thermogravimetric analyzer test (TGA). The test method is applicable to base stocks and fully formulated lubricant oils having a Noack evaporative loss ranging from 0 % to 30 % by mass. This procedure requires much smaller specimens, and is faster when multiple samples are sequentially analyzed, and safer than the standard Noack method using Wood's metal.  
1.2 The evaporative loss determined by this test method is the same as that determined using the standard Noack test methods.  
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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products may contain acidic constituents that are present as additives, degradation products formed during service, such as oxidation products or components formed from combustion gases. The i-pH-value is a measure of the amount of acidic substances and their acidity defined under the conditions of test. The i-pH-value is used as a measure of lubricant degradation in service.  
5.2 The corrosiveness of acidic components depends on their concentration and acidity. The i-pH-value is a measure of the amount of dissociated acidic components with the potential of corrosiveness towards metals.  
5.3 Since a variety of oxidation and blow-by products contribute to the i-pH-value, this test method cannot be used to predict corrosiveness of oil or blends under service conditions against metallic components. No general correlation is known between i-pH-value and the corrosive tendency of blends or oils toward metals.
SCOPE
1.1 This test method covers procedures for the determination of initial pH (i-pH) in new and in-service lubricants.
Note 1: In new and used oils, the constituents that may be considered to have characteristics influencing the i-pH value include organic and inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, salts of ammonia and other weak bases, acid salts of polybasic acids, and addition agents such as inhibitors and detergents. “Initial” is used to differentiate from aqueous systems. The analysis is terminated after a defined time interval whenever equilibrium conditions, as known for pH measurements in aqueous systems, are not reached (see 3.1.1.2)  
1.2 This test method is used to indicate relative changes that occur in oil during use under oxidizing conditions or due to contamination by blow-by gases of combustion processes of biogases regardless of the color or other properties of the in-service lubricants. Although the initial pH is made under definite equilibrium conditions, the test method is not intended to measure an absolute acidic property that can be used to predict performance of oil under service conditions. No general correlation between corrosion of non-ferrous bearing metals and initial pH value is known.  
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.

SIGNIFICANCE AND USE
5.1 The carbon residue value of burner fuel serves as a rough approximation of the tendency of the fuel to form deposits in vaporizing pot-type and sleeve-type burners. Similarly, provided alkyl nitrates are absent (or if present, provided the test is performed on the base fuel without additive) the carbon residue of diesel fuel correlates approximately with combustion chamber deposits.  
5.2 The carbon residue value of motor oil, while at one time regarded as indicative of the amount of carbonaceous deposits a motor oil would form in the combustion chamber of an engine, is now considered to be of doubtful significance due to the presence of additives in many oils. For example, an ash-forming detergent additive can increase the carbon residue value of an oil yet will generally reduce its tendency to form deposits.  
5.3 The carbon residue value of gas oil is useful as a guide in the manufacture of gas from gas oil, while carbon residue values of crude oil residuum, cylinder and bright stocks, are useful in the manufacture of lubricants.
SCOPE
1.1 This test method covers the determination of the amount of carbon residue (Note 1) left after evaporation and pyrolysis of an oil, and it is intended to provide some indication of relative coke-forming propensity. This test method is generally applicable to relatively nonvolatile petroleum products which partially decompose on distillation at atmospheric pressure. This test method also covers the determination of carbon residue on 10 % (V/V) distillation residues (see Section 10). Petroleum products containing ash-forming constituents as determined by Test Method D482, will have an erroneously high carbon residue, depending upon the amount of ash formed (Notes 2 and 3).  
Note 1: The term carbon residue is used throughout this test method to designate the carbonaceous residue formed during evaporation and pyrolysis of a petroleum product. The residue is not composed entirely of carbon, but is a coke which can be further changed by pyrolysis. The term carbon residue is continued in this test method only in deference to its wide common usage.
Note 2: Values obtained by this test method are not numerically the same as those obtained by Test Method D189, or Test Method D4530. Approximate correlations have been derived (see Fig. X2.1) but need not apply to all materials which can be tested because the carbon residue test is applicable to a wide variety of petroleum products. The Ramsbottom Carbon Residue test method is limited to those samples that are mobile below 90 °C.
Note 3: In diesel fuel, the presence of alkyl nitrates such as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon residue value than observed in untreated fuel, which can lead to erroneous conclusions as to the coke-forming propensity of the fuel. The presence of alkyl nitrate in the fuel can be detected by Test Method D4046.
Note 4: The test procedure in Section 10 is being modified to allow the use of a 100 mL volume automated distillation apparatus. No precision data is available for the procedure at this time, but a round robin is being planned to develop precision data. The 250 mL volume bulb distillation method described in Section 10 for determining carbon residue on a 10 % distillation residue is considered the referee test.  
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 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...

SIGNIFICANCE AND USE
5.1 Blends of fuel ethanol and hydrocarbon have a limited solvency for water that is dependent upon temperature and the ratio of ethanol to hydrocarbon. Good handling practices are important during the blending, storage, and transportation of fuel to avoid water contamination. High concentrations of water can cause haze or phase separation in ethanol and hydrocarbon blends and lead to freezing problems at low temperatures. Water has also been associated with corrosion and filter plugging.
SCOPE
1.1 This test method covers the determination of water in blends of ethanol, hydrocarbon, and corresponding blends. It is intended for measuring water content of gasoline or other hydrocarbon blendstock, denatured fuel ethanol as cited in Specification D4806, and ethanol fuel blends such as those cited in Specification D5798 and Practice D7794. This test method is not applicable to samples that are phase separated.  
1.1.1 Procedure A—For measurement of water from 0.004 % by mass to 1.63 % by mass in ethanol and hydrocarbon using coulometric Karl Fischer titration. This is the referee method for samples containing up to 1.63 % water.  
1.1.2 Procedure B—For measurement of water from 0.02 % by mass to 5.41 % by mass in ethanol and hydrocarbon using volumetric Karl Fischer titration.  
1.2 This method measures mass percent water and allows for the alternative reporting of volume percent. This test method recommends the use of pyridine-free reagents.  
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. Specific precautionary statements are given in Section 8.  
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.

SIGNIFICANCE AND USE
5.1 Coagulated pentane insolubles can include oil-insoluble materials, some oil-insoluble resinous matter originating from oil or additive degradation, soot from incomplete diesel fuel combustion, or a combination of all three.  
5.2 A significant change in coagulated pentane insolubles indicates a change in oil, and this could lead to lubrication system problems.  
5.3 Coagulated pentane insolubles measurements can also assist in evaluating the performance characteristics of a used oil or in determining the cause of equipment failure.  
5.4 High values of coagulated pentane insolubles have been associated with plugged oil filters, leading to opening of the bypass valve and circulation of unfiltered oil in the engine. This can lead to increased piston deposits, increased bearing wear, and premature engine failure.
SCOPE
1.1 This test method covers the determination of coagulated pentane insolubles in used lubricating oils by a paper filtration method.  
1.2 This test method was originally developed by the Fuels, Lubricants, and Environmental Committee (FL&E) of the Locomotive Maintenance Officer’s Association (LMOA).2  
1.3 This test method is used primary for testing used diesel engine oils from railroad locomotive service. It may be applied to other samples types but precision, bias, and significance have not been determined for samples other than used railroad locomotive diesel engine oils.  
1.4 This test method, in general, does not correlate with Test Method D893 on Insolubles in Lubricating Oils, since it uses separation by centrifugation and a more concentrated solution of anti-coagulant.  
1.5 The correlation between this test method and Appendix A4 (Enhanced Thermal Gravimetric Analysis (TGA) Procedure) in Test Method D5967 has not been investigated.  
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. For specific warning statements, see 7.2, 7.3, and 7.4.  
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.

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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 Pyrolysis liquid can be produced to various char concentrations. Increasing pyrolysis solids content can affect the pyrolysis liquid biofuel handling, atomization and storage stability in a negative manner.
SCOPE
1.1 This test method describes a filtration procedure for determining the pyrolysis solids content of pyrolysis liquid. It is intended for the analysis of pyrolysis liquid with all ranges of pyrolysis solids concentrations.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage. For specific warning statements, see 7.2, 7.3, and 7.4.  
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.

SIGNIFICANCE AND USE
5.1 Pentane insolubles above 0.8 μm in size may lead to increased wear. This increased wear can lead to premature equipment failure in critical applications.
SCOPE
1.1 This test method covers the determination of pentane insolubles for particles exceeding 0.8 μm in new and used lubricating oils.  
Note 1: Pentane insolubles with particle sizes less than 0.8 μm may be studied with appropriate size membrane filters. Particle sizes above or below 0.8 μm can be studied. The precision of this test method has been determined only at 0.8 μm.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  For specific warning statements, see 7.1, 8.2.1, and Annex A1.  
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.

SIGNIFICANCE AND USE
4.1 This test method is a means for ascertaining whether pharmaceutical mineral oil conforms to the standards of the United States Pharmacopeia, the National Formulary, and the Food and Drug Administration.
SCOPE
1.1 This test method covers white mineral oil (Mineral Oil USP and Light Mineral Oil NF) to determine whether it conforms to the standard of quality required for pharmaceutical use as defined by the United States Pharmacopeia and the National Formulary, or the Food and Drug Administration.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 Exception—Dimension requirements for the color comparator in Fig. 1 are in SI and inch-pound units.  
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 6.  
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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products, biodiesel, and blends of biodiesel may contain 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 bases. The acid number is a measure of this amount of acidic substance in the oil, always under the conditions of the test. The acid 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. Any condemning limits must be empirically established.  
5.2 Since a variety of oxidation products contribute to the acid number and the organic acids vary widely in corrosion properties, the test method cannot be used to predict corrosiveness of oil or biodiesel and blends under service conditions. No general correlation is known between acid number and the corrosive tendency of biodiesel and blends or oils toward metals.
SCOPE
1.1 This test method covers procedures for the determination of acidic constituents in petroleum products, lubricants, biodiesel, and blends of biodiesel.  
1.1.1 Test Method A—For petroleum products and lubricants soluble or nearly soluble in mixtures of toluene and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. Salts react if their hydrolysis constants are larger than 10–9. The range of acid numbers included in the precision statement is 0.1 mg/g KOH to 150 mg/g KOH.  
1.1.2 Test Method B—Developed specifically for biodiesel and biodiesel blends with low acidity and slightly different solubility. This test method requires the use of an automatic titrator with automatic endpoint-seeking capability.
Note 1: In new and used oils, the constituents that may be considered to have acidic characteristics include organic and inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, salts of ammonia and other weak bases, acid salts of polybasic acids, and addition agents such as inhibitors and detergents.  
1.2 The test method may be used to indicate relative changes that occur in oil during use under oxidizing conditions regardless of the color or other properties of the resulting oil. Although the titration is made under definite equilibrium conditions, the test method is not intended to measure an absolute acidic property that can be used to predict performance of oil under service conditions. No general relationship between bearing corrosion and acid number is known.
Note 2: The acid number obtained by this standard may or may not be numerically the same as that obtained in accordance with Test Methods D974 and D3339. There has not been any attempt to correlate this method with other non-titration methods.
Note 3: A few laboratories have made the observation that there is a difference in Test Method D664 results when aqueous versus nonaqueous buffers are used.  
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.

SIGNIFICANCE AND USE
5.1 This test method is useful for distinguishing between oils that are adaptable to various types of spraying application, with a higher unsulfonated oil being required for leaf spraying as compared to dormant vegetation application.
SCOPE
1.1 This test method covers the determination of unsulfonated residue in plant spray oils of petroleum origin and applies only to the petroleum oil content. It provides a measure of the degree of refinement of plant spray oils by determining the extent to which the oil is attacked by 98.61 % sulfuric acid under closely standardized conditions. Since the relationship between unsulfonated residue and the actual composition of the oil is not known, this test method should be applied only for measuring the degree of refinement and not for the determination of aromatics or olefins, or both.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 Pentane insolubles can include oil-insoluble materials and some oil-insoluble resinous matter originating from oil or additive degradation, or both.  
5.2 Toluene insoluble materials can come from (1) external contamination, (2) fuel carbon and highly carbonized materials from degradation of fuel, oil, and additives, or (3) engine wear and corrosion materials.  
5.3 A significant change in pentane insolubles, toluene insolubles (with or without coagulant), and insoluble resins indicates a change in oil which could lead to lubrication system problems.  
5.4 Insolubles measured can also assist in evaluating the performance characteristics of a used oil or in determining the cause of equipment failure.
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 SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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. For specific warning statements, see Section 7 and 9.1.1.  
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.

SIGNIFICANCE AND USE
5.1 Petroleum products can contain additives that react with alkali to form metal soaps. Fats are examples of such additives. Also, certain used engine oils, especially from turbine or internal combustion engines, can contain chemicals that will similarly react with alkali. The saponification number expresses the amount of base that will react with 1 g of sample when heated in a specific manner. This then gives an estimation of the amount of acid present in the sample, that is, any free acid originally present plus any combined (for example, in esters) that have been converted to metal soaps during the heating procedure.  
5.2 Saponification numbers are also used in setting product specifications for lubricants and additives.
SCOPE
1.1 These test methods cover the determination of the amount of constituents in petroleum products such as lubricants, additives, and transmission fluids that will saponify under the conditions of the test.  
Note 1: Statements defining this test and its significance when applied to electrical insulating oils of mineral origin will be found in Guide D117. Experience has shown that for transformer oils, Test Method D94, modified by use of 0.1  M KOH solution and 0.1 M HCl, is more suitable.  
1.1.1 Two test methods are described: Method A—Color Indicator Titration (Sections 6 – 13), and Method B—Potentiometric Titration (Sections 14 – 23).  
1.2 Because compounds of sulfur, phosphorus, the halogens, and certain other elements that are sometimes added to petroleum products also consume alkali and acids, the results obtained indicate the effect of these extraneous materials in addition to the saponifiable material present. Results on products containing such materials, on used internal-combustion-engine crankcase oils, and on used turbine oils must be interpreted with caution.  
Note 2: The materials referred to above, which are not normally considered saponifiable matter, include inorganic or certain organic acids, most nonalkali soaps, and so forth. The presence of such materials increases the saponification number above that of fatty saponifiable materials for which the test method is primarily intended. The odor of hydrogen sulfide near the end of the back-titration in the saponification test is an indication that certain types of reactive sulfur compounds are present in the sample. In the case of other reactive sulfur, chlorine, and phosphorus compounds and other interfering materials, no simple indication is given during the test. A gravimetric determination of the actual amount of fatty acids is probably the most reliable method for such compounds. Test Methods D128 or IP Method 284/86 can be used to determine fatty acids gravimetrically.  
1.3 The values stated in 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. For specific hazard statements, see Sections 6, 7, 8, 10, 15, 16, 17, and 19.  
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.

SIGNIFICANCE AND USE
5.1 The tendency of oils to foam at high temperature can be a serious problem in systems such as high-speed gearing, high volume pumping, and splash lubrication. Foaming can cause inadequate lubrication, cavitation, and loss of lubricant due to overflow, and these events can lead to mechanical failure.  
5.2 Correlation between the amount of foam created or the time for foam to collapse, or both, and actual lubrication failure has not been established. Such relations should be empirically determined for foam sensitive applications.
SCOPE
1.1 This test method covers the procedure for determining the foaming characteristics of lubricating oils (specifically transmission fluid and motor oil) at 150 °C.  
1.2 Foaming characteristics of lubricating oils at temperatures up to 93.5 °C are determined by Test Method D892 or IP 146.  
1.3 The values stated in SI units are to be regarded as standard.  
1.3.1 Exception—The values given in parentheses are provided for information only.  
1.4 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.  
1.5 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.  
1.6 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.

SIGNIFICANCE AND USE
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.  
5.2 Since a variety of oxidation products contribute to the acid number and the organic acids vary widely in corrosive properties, the test cannot be used to predict corrosiveness of an oil under service conditions. No general correlation is known between acid number and the corrosive tendency of oils toward metals. Compounded engine oils can and usually do have both acid and base numbers in this test method.
SCOPE
1.1 This test method covers the determination of acidic or basic constituents (Note 1) in petroleum products2 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.
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 D4739 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 D664. The acid numbers obtained by this color-indicator test method need not be numerically the same as those obtained by Test Method D664, the base numbers obtained by this color indicator test method need not be numerically the same as those obtained by Test Method D4739, but they are generally of the same order of magnitude.  
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...

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 The apparatuses used in Procedure C (see Annex A2) and Procedure D, also permit 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 four procedures for determining the evaporation loss of lubricating oils (particularly engine oils). The evaporation measured is reported as percent total loss. The test method relates to one set of operating conditions but may be readily adapted to other conditions as required.  
1.2 Procedure B and Procedure D that are in the main section of the test method provide equivalent results. Procedures A and C , which are in Annex A1 and Annex A2, have equivalent results. It has been determined that Procedures A and C show a slight bias when compared to Procedures B and D. Procedures B and D give slightly higher results versus Procedures A and C on formulated engine oils, while Procedures B and D give lower results versus Procedures A and C on basestocks. Thus, a correction factor is utilized to convert between the two sets of Procedures based on the fluid type.  
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.

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 The apparatuses used in Procedure C (see Annex A2) and Procedure D, also permit 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 four procedures for determining the evaporation loss of lubricating oils (particularly engine oils). The evaporation measured is reported as percent total loss. The test method relates to one set of operating conditions but may be readily adapted to other conditions as required.  
1.2 Procedure B and Procedure D that are in the main section of the test method provide equivalent results. Procedures A and C , which are in Annex A1 and Annex A2, have equivalent results. It has been determined that Procedures A and C show a slight bias when compared to Procedures B and D. Procedures B and D give slightly higher results versus Procedures A and C on formulated engine oils, while Procedures B and D give lower results versus Procedures A and C on basestocks. Thus, a correction factor is utilized to convert between the two sets of Procedures based on the fluid type.  
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.

SIGNIFICANCE AND USE
5.1 The carbon residue value of burner fuel serves as a rough approximation of the tendency of the fuel to form deposits in vaporizing pot-type and sleeve-type burners. Similarly, provided alkyl nitrates are absent (or if present, provided the test is performed on the base fuel without additive) the carbon residue of diesel fuel correlates approximately with combustion chamber deposits.  
5.2 The carbon residue value of motor oil, while at one time regarded as indicative of the amount of carbonaceous deposits a motor oil would form in the combustion chamber of an engine, is now considered to be of doubtful significance due to the presence of additives in many oils. For example, an ash-forming detergent additive may increase the carbon residue value of an oil yet will generally reduce its tendency to form deposits.  
5.3 The carbon residue value of gas oil is useful as a guide in the manufacture of gas from gas oil, while carbon residue values of crude oil residuums, cylinder and bright stocks, are useful in the manufacture of lubricants.
SCOPE
1.1 This test method covers the determination of the amount of carbon residue (Note 1) left after evaporation and pyrolysis of an oil, and is intended to provide some indication of relative coke-forming propensities. This test method is generally applicable to relatively nonvolatile petroleum products which partially decompose on distillation at atmospheric pressure. Petroleum products containing ash-forming constituents as determined by Test Method D482 or IP Method 4 will have an erroneously high carbon residue, depending upon the amount of ash formed (Note 2 and Note 4).  
Note 1: The term carbon residue is used throughout this test method to designate the carbonaceous residue formed after evaporation and pyrolysis of a petroleum product under the conditions specified in this test method. The residue is not composed entirely of carbon, but is a coke which can be further changed by pyrolysis. The term carbon residue is continued in this test method only in deference to its wide common usage.
Note 2: Values obtained by this test method are not numerically the same as those obtained by Test Method D524. Approximate correlations have been derived (see Fig. X1.1), but need not apply to all materials which can be tested because the carbon residue test is applied to a wide variety of petroleum products.
Note 3: The test results are equivalent to Test Method D4530, (see Fig. X1.2).
Note 4: In diesel fuel, the presence of alkyl nitrates such as amyl nitrate, hexyl nitrate, or octyl nitrate causes a higher residue value than observed in untreated fuel, which can lead to erroneous conclusions as to the coke forming propensity of the fuel. The presence of alkyl nitrate in the fuel can be detected by Test Method D4046.  
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 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.  
1.4 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 standardiza...

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 four 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; Procedure C uses Selby-Noack volatility test equipment, and Procedure D uses the Noack S2 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 C provide equivalent results and Procedures B and D provide equivalent results. However, A/C compared to B/D show consistent differences. Procedure A/C give slightly lower results versus Procedure B/D on formulated engine oils, while Procedure A/C give higher results versus Procedure B/D 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, 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.

SIGNIFICANCE AND USE
5.1 This test method provides a measure of trace amounts of unsaturated hydrocarbons in petroleum distillates boiling up to 288 °C (550 °F). An estimate of the quantity of these materials is useful in assessing the suitability of the lighter fractions for use as reaction solvents.
SCOPE
1.1 This test method covers the determination of the amount of bromine-reactive material in petroleum hydrocarbons and is thus a measure of trace amounts of unsaturates in these materials. It is applicable to materials having bromine indexes below 1000.  
1.2 This test method is applicable only to essentially olefin-free hydrocarbons or mixtures that are substantially free from material lighter than isobutane and have a distillation end point under 288 °C (550 °F).
Note 1: This procedure has been cooperatively tested on materials with bromine indexes in the range from 100 to 1000. These materials include petroleum distillates such as straight-run and hydrocracked naphtha, reformer feed, kerosine, and aviation turbine fuel.
Note 2: Materials with bromine index greater than 1000 should be tested for bromine number using Test Method D1159/IP 130.
Note 3: Bromine index of industrial aromatic hydrocarbons should be determined using Test Method D1492 or D5776. The subcommittee is currently examining ways to achieve more consistent end point values.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products, biodiesel, and blends of biodiesel may contain 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 bases. The acid number is a measure of this amount of acidic substance in the oil, always under the conditions of the test. The acid 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. Any condemning limits must be empirically established.  
5.2 Since a variety of oxidation products contribute to the acid number and the organic acids vary widely in corrosion properties, the test method cannot be used to predict corrosiveness of oil or biodiesel and blends under service conditions. No general correlation is known between acid number and the corrosive tendency of biodiesel and blends or oils toward metals.
SCOPE
1.1 This test method covers procedures for the determination of acidic constituents in petroleum products, lubricants, biodiesel, and blends of biodiesel.  
1.1.1 Test Method A—For petroleum products and lubricants soluble or nearly soluble in mixtures of toluene and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. Salts react if their hydrolysis constants are larger than 10–9. The range of acid numbers included in the precision statement is 0.1 mg/g KOH to 150 mg/g KOH.  
1.1.2 Test Method B—Developed specifically for biodiesel and biodiesel blends with low acidity and slightly different solubility. This test method requires the use of an automatic titrator with automatic endpoint-seeking capability.
Note 1: In new and used oils, the constituents that may be considered to have acidic characteristics include organic and inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, salts of ammonia and other weak bases, acid salts of polybasic acids, and addition agents such as inhibitors and detergents.  
1.2 The test method may be used to indicate relative changes that occur in oil during use under oxidizing conditions regardless of the color or other properties of the resulting oil. Although the titration is made under definite equilibrium conditions, the test method is not intended to measure an absolute acidic property that can be used to predict performance of oil under service conditions. No general relationship between bearing corrosion and acid number is known.
Note 2: The acid number obtained by this standard may or may not be numerically the same as that obtained in accordance with Test Methods D974 and D3339. There has not been any attempt to correlate this method with other non-titration methods.
Note 3: A few laboratories have made the observation that there is a difference in Test Method D664 results when aqueous versus nonaqueous buffers are used.  
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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products, biodiesel, and blends of biodiesel may contain 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 bases. The acid number is a measure of this amount of acidic substance in the oil, always under the conditions of the test. The acid 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. Any condemning limits must be empirically established.  
5.2 Since a variety of oxidation products contribute to the acid number and the organic acids vary widely in corrosion properties, the test method cannot be used to predict corrosiveness of oil or biodiesel and blends under service conditions. No general correlation is known between acid number and the corrosive tendency of biodiesel and blends or oils toward metals.
SCOPE
1.1 This test method covers procedures for the determination of acidic constituents in petroleum products, lubricants, biodiesel, and blends of biodiesel.  
1.1.1 Test Method A—For petroleum products and lubricants soluble or nearly soluble in mixtures of toluene and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. Salts react if their hydrolysis constants are larger than 10–9. The range of acid numbers included in the precision statement is 0.1 mg/g KOH to 150 mg/g KOH.  
1.1.2 Test Method B—Developed specifically for biodiesel and biodiesel blends with low acidity and slightly different solubility. This test method requires the use of an automatic titrator with automatic endpoint-seeking capability.
Note 1: In new and used oils, the constituents that may be considered to have acidic characteristics include organic and inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, salts of ammonia and other weak bases, acid salts of polybasic acids, and addition agents such as inhibitors and detergents.  
1.2 The test method may be used to indicate relative changes that occur in oil during use under oxidizing conditions regardless of the color or other properties of the resulting oil. Although the titration is made under definite equilibrium conditions, the test method is not intended to measure an absolute acidic property that can be used to predict performance of oil under service conditions. No general relationship between bearing corrosion and acid number is known.
Note 2: The acid number obtained by this standard may or may not be numerically the same as that obtained in accordance with Test Methods D974 and D3339. There has not been any attempt to correlate this method with other non-titration methods.
Note 3: A few laboratories have made the observation that there is a difference in Test Method D664 results when aqueous versus nonaqueous buffers are used.  
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.

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 four 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; Procedure C uses Selby-Noack volatility test equipment, and Procedure D uses the Noack S2 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 C provide equivalent results and Procedures B and D provide equivalent results. However, A/C compared to B/D show consistent differences. Procedure A/C give slightly lower results versus Procedure B/D on formulated engine oils, while Procedure A/C give higher results versus Procedure B/D 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, 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.

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 four 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; Procedure C uses Selby-Noack volatility test equipment, and Procedure D uses the Noack S2 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 C provide equivalent results and Procedures B and D provide equivalent results. However, A/C compared to B/D show consistent differences. Procedure A/C give slightly lower results versus Procedure B/D on formulated engine oils, while Procedure A/C give higher results versus Procedure B/D 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, 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.

SIGNIFICANCE AND USE
5.1 The tendency of oils to foam can be a serious problem in systems such as high-speed gearing, high-volume pumping, and splash lubrication. Inadequate lubrication, cavitation, and overflow loss of lubricant can lead to mechanical failure. This test method is used in the evaluation of oils for such operating conditions.
SCOPE
1.1 This test method covers the determination of the foaming characteristics of lubricating oils at 24 °C and 93.5 °C. Means of empirically rating the foaming tendency and the stability of the foam are described.  
1.2 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.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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. For specific warning statements, see Sections 7, 8, and 9.1.1.  
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.

SIGNIFICANCE AND USE
5.1 The tendency of oils to foam can be a serious problem in systems such as high-speed gearing, high-volume pumping, and splash lubrication. Inadequate lubrication, cavitation, and overflow loss of lubricant can lead to mechanical failure. This test method is used in the evaluation of oils for such operating conditions.
SCOPE
1.1 This test method covers the determination of the foaming characteristics of lubricating oils at 24 °C and 93.5 °C. Means of empirically rating the foaming tendency and the stability of the foam are described.  
1.2 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.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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. For specific warning statements, see Sections 7, 8, and 9.1.1.  
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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products, biodiesel, and blends of biodiesel may contain 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 bases. The acid number is a measure of this amount of acidic substance in the oil, always under the conditions of the test. The acid 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. Any condemning limits must be empirically established.  
5.2 Since a variety of oxidation products contribute to the acid number and the organic acids vary widely in corrosion properties, the test method cannot be used to predict corrosiveness of oil or biodiesel and blends under service conditions. No general correlation is known between acid number and the corrosive tendency of biodiesel and blends or oils toward metals.
SCOPE
1.1 This test method covers procedures for the determination of acidic constituents in petroleum products, lubricants, biodiesel, and blends of biodiesel.  
1.1.1 Test Method A—For petroleum products and lubricants soluble or nearly soluble in mixtures of toluene and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. Salts react if their hydrolysis constants are larger than 10–9. The range of acid numbers included in the precision statement is 0.1 mg/g KOH to 150 mg/g KOH.  
1.1.2 Test Method B—Developed specifically for biodiesel and biodiesel blends with low acidity and slightly different solubility. This test method requires the use of an automatic titrator with automatic endpoint-seeking capability.
Note 1: In new and used oils, the constituents that may be considered to have acidic characteristics include organic and inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, salts of ammonia and other weak bases, acid salts of polybasic acids, and addition agents such as inhibitors and detergents.  
1.2 The test method may be used to indicate relative changes that occur in oil during use under oxidizing conditions regardless of the color or other properties of the resulting oil. Although the titration is made under definite equilibrium conditions, the test method is not intended to measure an absolute acidic property that can be used to predict performance of oil under service conditions. No general relationship between bearing corrosion and acid number is known.
Note 2: The acid number obtained by this standard may or may not be numerically the same as that obtained in accordance with Test Methods D974 and D3339. There has not been any attempt to correlate this method with other non-titration methods.
Note 3: A few laboratories have made the observation that there is a difference in Test Method D664 results when aqueous versus nonaqueous buffers are used.  
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.

SIGNIFICANCE AND USE
5.1 New and used petroleum products can contain basic constituents that are present as additives. The relative amount of these materials can be determined by titration with acids. The base number is a measure of the amount of basic substances in the oil always under the conditions of the test. It is sometimes used as a measure of lubricant degradation in service. However, any condemning limit shall be empirically established.  
5.2 As stated in 1.2, this test method uses a weaker acid to titrate the base than Test Method D2896, and the titration solvents are also different. Test Method D2896 uses a stronger acid and a more polar solvent system than Test Method D4739. As a result, Test Method D2896 will titrate salts of weak acids (soaps), basic salts of polyacidic bases, and weak alkaline salts of some metals. They do not protect the oil from acidic components due to the degradation of the oil. This test method may produce a falsely exaggerated base number. Test Method D4739 will probably not titrate these weak bases but, if so, will titrate them to a lesser degree of completion. It measures only the basic components of the additive package that neutralizes acids. On the other hand, if the additive package contains weak basic components that do not play a role in neutralizing the acidic components of the degrading oil, then the Test Method D4739 result may be falsely understated.  
5.3 Particular care is required in the interpretation of the base number of new and used lubricants.  
5.3.1 When the base number of the new oil is required as an expression of its manufactured quality, Test Method D2896 is preferred, since it is known to titrate weak bases that this test method may or may not titrate reliably.  
5.3.2 When the base number of in-service or at-term oil is required, this test method is preferred because in many cases, especially for internal combustion engine oils, weakly basic degradation products are possible. Test Method D2896 will titrate these, thu...
SCOPE
1.1 This test method covers a procedure for the determination of basic constituents in petroleum products and new and used lubricants. This test method resolves these constituents into groups having weak-base and strong-base ionization properties, provided the dissociation constants of the more strongly basic compounds are at least 1000 times than that of the next weaker groups. This test method covers base numbers up to 250.  
1.2 In new and used lubricants, the constituents that can be considered to have basic properties are primarily organic and inorganic bases, including amino compounds. This test method uses hydrochloric acid as the titrant, whereas Test Method D2896 uses perchloric acid as the titrant. This test method may or may not titrate these weak bases and, if so, it will titrate them to a lesser degree of completion; some additives such as inhibitors or detergents may show basic characteristics.  
1.3 When testing used engine lubricants, it should be recognized that certain weak bases are the result of the service rather than having been built into the oil. This test method can be used to indicate relative changes that occur in oil during use under oxidizing or other service conditions regardless of the color or other properties of the resulting oil. The values obtained, however, are intended to be compared with the other values obtained by this test method only; base numbers obtained by this test method are not intended to be equal to values by other test methods. Although the analysis is made under closely specified conditions, this test method is not intended to, and does not, result in reported basic properties that can be used under all service conditions to predict performance of an oil; for example, no overall relationship is known between bearing corrosion or the control of corrosive wear in the engine and base number.  
1.4 This test method was developed as an alternative for the former base numb...

SIGNIFICANCE AND USE
5.1 New and used petroleum products, biodiesel, and blends of biodiesel may contain 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 bases. The acid number is a measure of this amount of acidic substance in the oil, always under the conditions of the test. The acid 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. Any condemning limits must be empirically established.  
5.2 Since a variety of oxidation products contribute to the acid number and the organic acids vary widely in corrosion properties, the test method cannot be used to predict corrosiveness of oil or biodiesel and blends under service conditions. No general correlation is known between acid number and the corrosive tendency of biodiesel and blends or oils toward metals.
SCOPE
1.1 This test method covers procedures for the determination of acidic constituents in petroleum products, lubricants, biodiesel, and blends of biodiesel.  
1.1.1 Test Method A—For petroleum products and lubricants soluble or nearly soluble in mixtures of toluene and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. Salts react if their hydrolysis constants are larger than 10–9. The range of acid numbers included in the precision statement is 0.1 mg/g KOH to 150 mg/g KOH.  
1.1.2 Test Method B—Developed specifically for biodiesel and biodiesel blends with low acidity and slightly different solubility. This test method requires the use of an automatic titrator with automatic endpoint-seeking capability.
Note 1: In new and used oils, the constituents that may be considered to have acidic characteristics include organic and inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, salts of ammonia and other weak bases, acid salts of polybasic acids, and addition agents such as inhibitors and detergents.  
1.2 The test method may be used to indicate relative changes that occur in oil during use under oxidizing conditions regardless of the color or other properties of the resulting oil. Although the titration is made under definite equilibrium conditions, the test method is not intended to measure an absolute acidic property that can be used to predict performance of oil under service conditions. No general relationship between bearing corrosion and acid number is known.
Note 2: The acid number obtained by this standard may or may not be numerically the same as that obtained in accordance with Test Methods D974 and D3339. There has not been any attempt to correlate this method with other non-titration methods.
Note 3: A few laboratories have made the observation that there is a difference in Test Method D664 results when aqueous versus nonaqueous buffers are used.  
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.

SIGNIFICANCE AND USE
5.1 Crude oils and oil sands bitumen contain naturally occurring acidic species. Acidity of crude oil has been implicated in corrosion of distribution and process systems. The relative amount of these materials can be determined by titrating with bases. The acid number is a measure of this amount of acidic substance in the oil under the conditions of the test.  
5.2 Acid number of crude and distilled petroleum fractions has been measured by Test Method D664. Test Method D664 was developed for the analysis of lubricants and biodiesel. The titration solvent used in Test Method D664 does not properly address dissolving difficult samples such as crude oil, bitumen, and high wax samples addressed in this test method. Refer to Appendix X1.  
5.3 Test Method D974 is also not applicable to measuring acidity of crudes and highly colored samples because the indicator is not visible or it is difficult to discern a color change to detect the end point of the titration.
SCOPE
1.1 This test method covers the determination of acidic components in crude oil and petroleum products including waxes, bitumen, base stocks, and asphalts that are soluble in mixtures of xylenes and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. The values obtained by this test method may not be numerically equivalent to other acid value measurements. The range of KOH acid numbers included in the precision statement is 0.1 mg/g to 16 mg/g.  
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. Some specific hazards statements are given in Section 7 on Safety Precautions.  
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.