D01.34 - Pine Chemicals and Hydrocarbon Resins

SIGNIFICANCE AND USE
4.1 This is a revision of the method for measuring rosin acids content combines the three major ways of determining the rosin acids content of pine chemicals products into a single method.  
4.1.1 For materials containing less than 15 % rosin, the modified Glidden procedure has gained acceptance. For materials containing more than 15 % rosin the modified Wolfe Method is preferred. The modified Wolfe and modified Glidden procedures differ only in their details. They have been combined here into a single procedure. This procedure can be run using either a potentiometer or an internal indicator to determine the end point of the titration. Use of a potentiometer is preferred and is the referee method. Use of an internal indicator is the principal alternative method. They will be referred to as the Potentiometric Method and the Internal Indicator Method.
SCOPE
1.1 These test methods cover the determination of rosin acids in tall oil, tall oil fatty acid, tall oil rosin, and other pine chemicals products.  
1.2 These test methods may not be applicable to adducts or derivatives of rosin, fatty acid, or other pine chemicals products.  
1.3 The values stated in SI units are to be regarded as the standard. 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 Earlier methods for characterizing turpentine and related terpene products were based on physical properties, such as those in Specification D13 and Test Methods D801 and D802, and packed column gas chromatography for the major constituents (for example, α-pinene, β-pinene) as in Test Method D3009. As terpene products became widely used as chemical raw material, the separation and quantitation of compounds present at lower concentrations in the product became more important. The capillary gas chromatographic technique described in these test methods is a rapid and convenient means to perform these analyses.
SCOPE
1.1 These test methods describe the determination of the amounts of α-pinene, β-pinene, dipentene, terpene alcohols, and other terpene compounds in turpentine and related terpene products using capillary gas chromatography. The two methods for determining the amount of the individual terpene compounds are the “internal standard” method, which yields absolute values, and the “area percent” method, which yields relative values.  
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 the standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: Overall this test method gives excellent repeatability but only moderate reproducibility. This greater than normal differential is a consequence of the variety of gas chromatography (GC) columns and other variables used by participants. These variables, coupled with the complex composition of the test products, enabled some workers to separate peaks that others reported as one peak; thus, this test method gives excellent precision within a given laboratory on a given GC. When laboratory to laboratory comparison have to be made, however, it is essential that the GC operating conditions be defined closely.  
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 provides a more precise way of measuring Gardner color than described in Test Method D1544. It is applicable to rosin products having colors from Gardner 1 to Gardner 18. The Gardner scale is not applicable to materials with colors lighter than 1 or darker than 18.
SCOPE
1.1 This test method covers the quantitative determination of the color of clear, yellow/brown, liquid materials using color measuring instruments. The results may be invalid if other materials are used. The test uses the Gardner color scale described in Test Method D1544. This test method applies to pine chemical products including tall oil rosin, gum rosin, wood rosin and related products.  
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
3.1 Rosin and similar materials such as rosin derivatives often contain volatile material derived from the raw material used or formed as a result of the processing of the rosin. This volatile material can have a significant effect on the physical and chemical properties of the rosin and so a standard method for its determination is required.
SCOPE
1.1 This test method covers the determination of the volatile oil content of rosin or similar material. The oil may consist of naturally occurring terpene oil, such as heavy fractions of turpentine, resulting from incomplete distillation in the processing of the rosin, or of foreign nonterpene oil resulting from incomplete removal of mineral or coal-tar solvent used to extract the rosin from wood or still wastes. In certain cases the volatile oil could consist of decarboxylated rosin formed during the processing of the rosin.  
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
4.1 In general, with materials of these types, softening point does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results obtained are to be comparable.
SCOPE
1.1 This test method covers the determination of softening point of resins using a Mettler cup and ball apparatus, and may, under user-defined conditions, give results comparable to those obtained by Test Methods E28.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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
3.1 The iodine value of a fatty acid product is a measure of the unsaturated fatty acid content of that product and consequently a measure of the ease of oxidation or drying capacity of that fatty acid product.  
3.2 This test method measures the unsaturation as iodine value by addition of an iodine/chlorine reagent. The amount of reagent absorbed is determined by back titrating the excess reagent and comparing it to a blank determination.  
3.3 In samples containing conjugated double bonds, the iodine value obtained is empirical since the reagent does not react stoichiometrically with conjugated unsaturation. Where no conjugation is present, the iodine value obtained is a measure of the total unsaturation. By using proper specimen weights, the empirical values obtained are useful for comparative purposes.  
3.4 This test method was developed in order to replace the hazardous solvent, carbon tetrachloride, used in Test Method D1959 with the less hazardous and more available solvents, iso-octane and cyclohexane. As data on the satisfactory use of other solvents becomes available, this test method will be amended to include those solvents.  
3.5 This test method should have applicability to fatty acids and oils other than tall oil fatty acid but that possibility has not been investigated.
SCOPE
1.1 This test method covers the Wijs procedure for determination of unsaturation (iodine value) of tall oil fatty acids.  
1.2 Iodine value is a measure of the unsaturation of oils and fatty acids and is expressed in terms of the number of centigrams of iodine per gram of sample (weight percent of absorbed iodine).  
1.3 When this test method is used to determine the iodine value of fatty acids having conjugated systems, the result is not a measure of total unsaturated, but rather is an empirical value that affords a comparison of unsaturation. Total unsaturation of conjugated systems may be measured in accordance with Test Method D1541.  
1.4 The test method described here is not reliable for tall oil fatty acids containing an appreciable quantity of rosin.  
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.6 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.  
1.7 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
3.1 This test method is designed to broaden the scope of the previous edition of the test method by the inclusion of tall oil and tall oil derived from products as test materials. Test Methods D803 currently includes a method for the determination of unsaponifiable matter.  
3.2 The amount of unsaponifiable matter in tall oil and other related products is important in characterizing such products as it indicates the level of nonacidic material, both free and combined, present in the test material. The unsaponifiable in naval stores products is primarily composed of higher molecular weight alcohols, sterols, and hydrocarbons.
SCOPE
1.1 This test method covers the determination of the percentage of material in pine chemicals products as defined in Terminology D804 including rosin, tall oil, and related products, other than insoluble dirt or similar visible foreign matter that does not yield a water-soluble soap when the sample is saponified with potassium hydroxide.  
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.
Note 1: It has been reported that this method may not be applicable to gum rosin, especially any gum rosin containing volatile terpenes. Volatile terpenes are by definition unsaponifiable matter, and can be lost under the drying conditions described in 8.4. The method is applicable to tall oil rosin and wood rosin as these rosins do not contain volatile terpenes.  
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 This test method is used to measure the apparent viscosity of hydrocarbon resins at elevated temperatures. Elevated temperature viscosity values of a hydrocarbon resin may be related to the properties of coatings, adhesives and the like, containing such a resin.  
5.2 For hydrocarbon resins, values of apparent viscosity will usually be a function of shear rate under the conditions of test. Although the type of viscometer described in this test method operates under conditions of relatively low shear rate, shear rate depends on the spindle and rotational speed selected for a determination; therefore, comparisons between apparent viscosity values should be made only for measurements made with similar viscometers under conditions of equivalent shear rate.
SCOPE
1.1 This test method covers the determination of the apparent viscosity of hydrocarbon resins having apparent viscosities up to 2,000,000 millipascal seconds (mPa·s) (Note 1) at temperatures up to 300 °C [572 °F].
Note 1: The SI unit of (dynamic) viscosity is the pascal second. The centipoise (cP) is one millipascal second (mPa·s) and is frequently used as a viscosity unit.  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
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 Thermal analysis provides a rapid method for determining transition temperatures in HC resins that possess them.  
5.2 This practice is useful for both quality assurance and research.
SCOPE
1.1 This practice covers determination of glass transition temperatures of hydrocarbon (HC) resins by differential scanning calorimetry (DSC).  
1.2 This practice is applicable to HC resins as defined in Terminology D6640. The normal operating temperature range is from the cryogenic region to approximately 180 °C. The temperature range can be extended.  
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 Further discussion of glass transition can be found in Test Method D3418, and Test Method E1356.  
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
3.1 The testing procedures described in these test methods have been in use for many years and emphasize the physical properties of pine oil rather than its chemical composition. Test Methods D6387 describe a capillary gas chromatography method which is suitable for determining both the major and minor components found in pine oils.
SCOPE
1.1 These test methods cover procedures for sampling and testing pine oils, and are applicable to both natural pine oils derived from pine stumps either by the steam and solvent process or by destructive distillation, and also to synthetic pine oils obtained by the chemical hydration of terpene hydrocarbons.  
1.2 The procedures given in these test methods appear in the following order:    
Section  
Sampling  
4  
Appearance  
5  
Color  
6  
Specific Gravity  
7  
Refractive Index  
8  
Composition  
9  
Moisture  
10  
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
4.1 For hydrocarbon resins and rosin based resins, softening does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle solids or very viscous liquids to less viscous liquids. For this reason, determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results obtained are to be comparable.
SCOPE
1.1 These test methods are intended for determining the softening point of hydrocarbon resins, rosin based resins and similar materials by means of an automated ring-and-ball apparatus. Portions are similar in technical content to the automated-apparatus versions of Test Methods D36, E28, and ISO 4625.  
1.1.1 The ring-and-ball softening point of a hydrocarbon resin and rosin based resins may also be determined with lower precision using the manual ring-and-ball softening point procedure in Test Methods E28.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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
3.1 The testing procedures described in these test methods have been in use for many years and emphasize the physical properties rather than the chemical composition of dipentene. These procedures were sufficient when dipentene was used primarily as a solvent. Currently, however, dipentene finds application as a chemical raw material and a knowledge of its chemical composition is therefore important. Test Methods D6387 describe a capillary gas chromatography method which is suitable for determining both the major and minor components found in dipentene.
SCOPE
1.1 These test methods cover procedures for sampling and testing dipentene and related terpene solvents, consisting chiefly of monocyclic terpene hydrocarbons distilling above the range for turpentine.  
1.2 The procedures given in these test methods appear in the following order:    
Section  
Sampling  
4  
Detection and Removal of Separated Water  
5  
Appearance  
6  
Color  
7  
Odor  
8  
Specific Gravity  
9  
Refractive Index  
10  
Composition  
11  
Flash Point  
12  
Moisture  
13  
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.

SCOPE
1.1 Although the pine chemical industry has been a continuing producer of chemical products for many centuries, the nature of the industry, its products, and its terminology have changed. In particular, the original practice of recovering pine chemical through the processing of the exudate from pine trees has been supplemented by their extraction by solvent products of the wood pulping industry. For many years the industry was known as the Naval Stores industry but that term has gradually been replaced by the more descriptive and meaningful term, Pine Chemicals Industry. Thus, this terminology contains some old terms now mostly of historic value, together with the terms of the modern pine chemical industry.2  
1.2 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
3.1 Saturated fatty acids solidify at a higher temperature than unsaturated fatty acids. This test method provides a means of measuring the solidification temperature of a sample containing both unsaturated and saturated fatty acids by cooling the specimen and measuring the temperature at which solidification occurs.  
3.2 Samples containing higher levels of saturated acids will have a higher titer (solidification temperature) than those with lower levels of saturated acids.  
3.3 Water present in the sample will raise the titer, so provisions are made in the test method to remove traces of moisture.
SCOPE
1.1 This test method covers the determination of the solidification (titer) point of fatty acids and is applicable to all fatty acids.  
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
3.1 In general, with materials of these types, softening does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results obtained are to be comparable.  
3.2 In these test methods, the softening point is defined as the temperature at which a disk of the sample held within a horizontal ring is forced downward a distance of 25.4 mm (1 in.) under the weight of a steel ball as the sample is heated at 5 °C/min in a water, glycerin, silicone oil, ethylene glycol/water or glycerin/water bath.  
3.3 The automatic method was chosen to be the reference method because a round robin demonstrated that it gave more precise results than the manual method.
SCOPE
1.1 These test methods are intended for determining the softening point of resins (including rosin and terpene resins) and similar materials by means of the ring-and-ball apparatus.  
Note 1: For testing asphalts, tars, and pitches, see Test Method D36.  
1.1.1 Test method using the automated ring and ball softening point apparatus is the reference method and the test method using the manual ring and ball method is an alternative method.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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
4.1 This test method provides a more precise way of measuring Gardner color than described in Test Method D1544. It is applicable to pine chemical products having colors from Gardner 1 to Gardner 18. The Gardner scale is not applicable to materials with colors lighter than 1 or darker than 18.
SCOPE
1.1 This test method covers the quantitative determination of the color of clear, yellow/brown, liquid materials using color measuring instruments. The results may be invalid if other materials are used. The test uses the Gardner color scale described in Test Method D1544. This test method applies to pine chemical products including tall oil, tall oil fatty acids, rosin, and related products.  
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
3.1 The test procedures described in this standard were developed when the chief use for turpentine was as a solvent. Currently however, the chief use for turpentine (and pinenes) is as raw materials for the production of resins and synthetic organic chemicals. Thus the chemical composition of turpentines and pinenes is extremely important and tests, in addition to the ones described in these test methods, are required in order to fully characterize turpentines and pinenes. The most widely used technique for determining the chemical composition of turpentines (and pinenes) is gas chromatography (see Test Methods D6387).
SCOPE
1.1 These test methods cover procedures for sampling and testing turpentine, as defined by the Code of Federal Regulations and Terminology D804. These test methods are also used for the sampling and testing of pinenes, the major components of most turpentines.  
1.2 These test methods primarily measure the physical rather than the chemical properties of turpentines and pinenes. As turpentines and pinenes are currently used chiefly as chemical raw materials for the production of resins and synthetic organic chemicals, chemical composition is also very important. Consequently, testing the chemical composition of turpentines and pinenes by gas chromatography has displaced these test methods to a large extent. (See for example Test Methods D6387.)  
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that 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
3.1 Many pine chemical products contain water as a result of the processes used for their production. Typically refined products such as terpenes, pine oil, tall oil fatty acids, and distilled tall oil contain only traces of water, but crude tall oil might contain 0.5 % to 2.5 % of water. Although the Karl Fischer and coulometric methods are most applicable to low levels of moisture, these can be and are used at higher levels. The azeotropic distillation method is generally used at higher levels.
SCOPE
1.1 These test methods cover the quantitative determination of dissolved or occluded water present in any proportion in liquid pine chemicals, such as turpentine, pinene, dipentene, pine oil, tall oil, and tall oil fatty acids. Three methods of moisture testing are included. The Karl Fisher titration method is the preferred method for testing tall oil, Test Methods D803.  
1.1.1 The Karl Fischer Titration method is based on the reaction between water and a complex reagent2 consisting of iodine, sulfur dioxide, pyridine, and methanol, whereby the iodine is converted to a colorless compound. The appearance of a persistent iodine color in the reaction mixture indicates the complete removal of free water by reaction with the reagent, and the endpoint may be measured colorimetrically. Automatic titrators find this endpoint by the restoration of a current strength when the resistance provided by the presence of water is eliminated. Amperometric automatic titrators find this endpoint by detecting the current flow that occurs once water is eliminated.  
1.1.2 The coulometric titration method determines water content by electronic integration of a current sufficient to generate the precise amount of iodine from the required reagent to react with the water in the sample.  
1.1.3 The azeotropic method utilizes the relatively low boiling point of water, as compared with other sample constituents, in a toluene or xylene matrix so that water is collected in a trap and measured.  
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
3.1 The color of a tall oil fatty acid is readily affected by heat and oxidization. Variations in degree of heat, time of heat, and exposure to atmosphere during heating have a marked effect on the color obtained; therefore, conformity to the equipment and procedure outlined in this test method is essential to accuracy and precision.
SCOPE
1.1 This test method covers the measurement of the Gardner color of tall oil fatty acids after heating in an atmosphere of nitrogen at 205°C for one or two hours, depending on whether its iodine value is over or under 15, respectively. The specimen may be heated using either an aluminum heating block or an oil bath. This method is applicable to all tall oil fatty acids. Applicability of this method to other types of fatty acids has not been determined.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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
3.1 Tall oil fractionated products derived from tall oil are important commercial materials, primarily composed of fatty acids and rosin acids, but also containing some neutral material (see Terminology D804). For many applications, it is necessary to know the level of the individual fatty acids and rosin acids present in these products. Gas chromatography has proven to be a useful tool for such determinations (see Test Methods D509), and capillary chromatography, described in these test methods, is considered to be the most effective gas chromatographic technique currently available. In particular situations, other techniques may be more suitable than gas chromatography. For example, the presence of fatty acid esters in the sample would result in transesterification during the derivatization step that may affect the results.  
3.2 Due to hydrogen bonding, unmodified tall oil fatty acids and rosin acids cannot be volatilized at atmospheric pressure without undergoing decomposition. So, it is necessary to convert the free acids to the more volatile and more stable methyl esters, prior to chromatographic separation.  
3.3 These test methods describe four ways to prepare methyl esters. The classic method is through the use of diazomethane, but diazomethane is a hazardous and toxic material, and so is no longer the preferred agent. The use of diazomethane is detailed in Appendix X1.  
3.3.1 TMAH causes isomerization of a sample’s di- and polyunsaturated fatty acids, when it is used in even a slight excess. This leads to inaccurate results for the individual fatty acid components. TMAH should be used for materials containing only rosin acids, or when the identification or quantitation of individual fatty acid components is not important.  
3.3.2 TMPAH is the recommended methylating agent when the identification or quantitation of individual di- and polyunsaturated fatty acids is required. TMPAH produces results that are very similar to those of diazomethane, but with...
SCOPE
1.1 These test methods cover the determination of the amounts of the individual fatty acids and rosin acids in fractionated tall oil products, using capillary gas chromatographic separation of the volatile methyl esters of these acids.  
1.2 Four methods for forming the methyl esters, and two methods for determining the amounts of the individual fatty acids and rosin acids are described.  
1.2.1 The classic method for the formation of methyl esters is through the use of diazomethane, but diazomethane is a hazardous and toxic material, and so is no longer the preferred reagent. The use of diazomethane is detailed in the Appendix. Methyl esters may be formed through the use of tetramethylammonium hydroxide (TMAH), trimethylphenylammonium hydroxide (TMPAH), or N,N-dimethylformamide dimethyl acetal (DMF-DMA).  
1.2.2 The two methods for determining the amount of the individual fatty acids and rosin acids are the “internal standard” method, which yields absolute values, and the “area percent” method, which yields relative values.  
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
3.1 Rosin is an important product of the centuries old Naval Stores industry, now known as the Pine Chemical industry, and is produced and consumed in many countries throughout the world. Consequently, reliable methods of sampling and grading rosin are necessary. The test methods based on the use of the USDA Official Standards described herein, were developed many years ago for the sampling and grading of rosin and are similar to those included in the Naval Stores Act.3  
3.2 Although these test methods based on the use of the USDA Official Standards are still applicable, many additional test methods are now used to grade rosin. In particular, the color of rosin is now more commonly reported using the Gardner color scale rather than the USDA Official Standards. In addition, Test Methods E28, D465, and D5974 are widely used to assess the quality of rosin in addition to the color grading methods described in this standard. The Naval Stores Act of 1923 established the methods for grading rosin and authorized the “Official Naval Stores Standard of the United States”. Based upon a request from the chairman of the ASTM D01.34 Pine Chemicals and Hydrocarbon Resins subcommittee requesting that the Gardner color scale be used for grading the color of rosin, a letter from the Food and Drug Administration was received and is archived in Pine Chemicals Association4 files. It documents a no-objection response to the request to use the Gardner color scale as a standard for grading rosin and rosin derivatives. The no-objection response was conditioned on having a reliable correlation between the USRG Scale (the “Official Naval Stores Standard of the United States”) and the Gardner Color Scale. A correlation study of color measurements on the Gardner Color Scale and the USRG Scale was carried out by scientists at Tintometer, Inc, Amesbury, England. The results of the correlation were submitted to the Food and Drug Administration as supporting evidence for the use of the Gardner Co...
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1.1 These test methods cover procedures for sampling and determining the grade of rosin delivered in commercial bags, barrels, drums or in molten form. Although developed for rosin, these methods can also be used for the grading of modified rosins and rosin based resins.
Note 1: All rosin sold in interstate commerce must be described by reference to the U. S. Standards for rosin, and is therefore subject to grading prior to such sale. The grading procedure described in these test methods is used for checking grades or regrading after the rosin has moved from the primary markets to distributing or consuming points.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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 MW averages and the MWD are important characteristics of a resin. They may be used for a variety of correlations for fundamental studies, processing, or product applications. The MW and MWD values may also be used for production quality control of resins.  
5.2 Limitations—Comparison of SEC molecular weight values should be made only if the data were obtained under identical chromatographic conditions.
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1.1 This practice covers the determination of apparent molecular weight (MW) averages and molecular weight distributions (MWD) for THF-soluble hydrocarbon, rosin and terpene resins by size-exclusion chromatography (SEC). This technique is not absolute; it requires calibration with standards of known molecular weight. This practice is applicable to resins containing molecular-weight components that have elution volumes falling within the elution volume range defined by polystyrene standards.
Note 1: SEC is also known as gel permeation chromatography (GPC).  
1.2 SEC systems employ low-volume liquid chromatography components and columns packed with relatively small (generally 3 to 20 μm) microporous particles. High-performance liquid chromatography instrumentation and automated data handling systems for data acquisition and processing are also required.  
1.3 The values stated in SI units are to be regarded as the standard. 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 practice is useful for both quality control and research.
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1.1 This practice covers determination of the color stability of a hydrocarbon resin by exposure to a specific temperature for a defined time period in a forced-draft oven.  
1.2 Color stability is measured by the change in color of the test resin, measured via the yellowness index color scale, in accordance with Practice E313, or the procedure for Gardner Color, Test Method D6166.  
1.3 The values stated in SI units are to be regarded as standard. 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
3.1 Rosin, particularly gum and wood rosin, occasionally contains small amounts of contamination such as sand, dirt or bark. Rosin derivatives occasionally contain traces of insoluble material as a result of the raw materials used in their production or they may be generated during the production process. In all instances the presence of such insoluble material should be minimal. This test method describes a rapid and reliable procedure for determining the amount of such insoluble matter. It is based on the knowledge that rosin and most of its derivatives are soluble in numerous organic solvents whereas most common contaminants are not. It is especially useful for internal quality control rather than sales specifications.
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1.1 This test method covers the determination of the amount of insoluble matter in rosin and rosin derivatives as described in Terminology D804.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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
3.1 Tall oil, both crude and refined, is an important by-product of the alkaline (kraft) pulping of pine wood. It consists primarily of fatty acids, resin acids, and neutral materials; the levels of these various components depend on factors such as the species of pine tree, geographic location, climate, etc.  
3.1.1 Tall oil is used primarily as a commercial source of fatty acids and rosin, and, therefore, reliable methods for the analysis of these components is necessary.
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1.1 These test methods cover the test procedures to be applied to whole tall oils or refined tall oils. Previous editions of these test methods have described test procedures that are used to test tall oil fatty acid, rosin, and other tall oil-derived products as well as test crude and refined tall oil. Consequently, these test methods are widely cited in reference books and industry literature for the testing of tall oil-derived products.  
1.1.1 In this current revision, procedural details of some of the often-cited test methods have been removed and the test methods consolidated with other existing test methods. In such cases the consolidated methods, applicable to all tall oil-derived products.  
1.2 The procedures appear in the following order:    
Physical Tests  
Sections  
Viscosity:  
Rotational Viscometer Method (Preferred Method)  
7  
Bubble Time Method  
8  
Flash Point  
9  
Color  
10  
Moisture:  
11  
Insoluble Matter  
12  
Ash  
13  
Chemical Analysis  
Acid Number  
16  
Saponification Number  
17  
Rosin Acids  
18  
Unsaponifiable Matter  
19  
Fatty Acids  
20  
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that 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
3.1 These test methods are designed to broaden the scope of the earlier editions of the test method by the inclusion of tall oil and tall oil derived products as test materials and will be referenced in Test Methods D803.  
3.2 The acid number is an important property of pine chemical products, such as tall oil, and the products obtained by the fractionation of tall oil. It is the test method widely used to determine the total free acid content of these products.  
3.3 The potentiometric test method should be used when the most reproducible results are required.
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1.1 These test methods are intended for determining the acid number of pine chemical products as defined in Terminology D804 including tall oil products, wood and gum rosin, and other related materials. These test methods may not be applicable to all modified rosin products. Two test methods are covered, as follows:  
1.1.1 Potentiometric method (referee), and  
1.1.2 Internal indicator method (alternate).  
1.2 The potentiometric method is suitable for use with both light- and dark-colored products. It should be considered the referee method. The internal indicator method is suitable for use only with light- and medium-colored products with a Gardner color of less than 12. It should be considered the alternate method.  
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
3.1 These test methods are designed to broaden the scope of the earlier editions of the test method by the inclusion of tall oil and tall oil derived products as test materials and is referenced in Test Methods D803.  
3.2 The saponification number is an important property of tall oil and the products obtained by the fractionation of tall oil. It is the test method widely used to determine the total acid content, both free and combined, of these products.  
3.3 The potentiometric test method should be used when the most reproducible results are required.
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1.1 These test methods cover the determination of the saponification number of tall oil and products obtained by the fractionation of tall oil such as rosin, fatty acids and distilled tall oil as defined in Terminology D804. These test methods are also applicable to gum and wood rosin. Two test methods are covered as follows:  
1.1.1 Test method using a potentiometric method, and  
1.1.2 Test method using an internal indicator method.  
1.2 The potentiometric method is suitable for use with both light- and dark-colored test samples. It should be considered the referee method. The internal indicator method is suitable for use only with light- and medium-colored test samples. It should be considered the alternate method.  
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
4.1 These test methods are designed to broaden the scope of the previous edition of these test methods by the inclusion of tall oil as a test material. Test Methods D803 currently includes methods for the determination of the rosin acid and fatty acid content of crude tall oil. Test Methods D803 references Test Method D1585.  
4.2 Rosin and tall oil are composed primarily of rosin acids and fatty acids, and the measurement of these components is important in establishing the composition of these materials.
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1.1 These test methods cover the determination of the fatty acids of pine chemicals, including rosin, tall oil, and related products.  
1.2 These test methods may not be applicable to adducts or derivatives of rosin or other pine chemical products.  
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 Earlier methods for characterizing turpentine and related terpene products were based on physical properties, such as those in Specification D13 and Test Methods D801 and D802, and packed column gas chromatography for the major constituents (for example, α-pinene, β-pinene) as in Test Method D3009. As terpene products became widely used as chemical raw material, the separation and quantitation of compounds present at lower concentrations in the product became more important. The capillary gas chromatographic technique described in these test methods is a rapid and convenient means to perform these analyses.
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1.1 These test methods describe the determination of the amounts of α-pinene, β-pinene, dipentene, terpene alcohols, and other terpene compounds in turpentine and related terpene products using capillary gas chromatography. The two methods for determining the amount of the individual terpene compounds are the “internal standard” method, which yields absolute values, and the “area percent” method, which yields relative values.  
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 the standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: Overall this test method gives excellent repeatability but only moderate reproducibility. This greater than normal differential is a consequence of the variety of gas chromatography (GC) columns and other variables used by participants. These variables, coupled with the complex composition of the test products, enabled some workers to separate peaks that others reported as one peak; thus, this test method gives excellent precision within a given laboratory on a given GC. When laboratory to laboratory comparison have to be made, however, it is essential that the GC operating conditions be defined closely.  
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
3.1 This test method is designed to broaden the scope of the previous edition of the test method by the inclusion of tall oil and tall oil derived from products as test materials. Test Methods D803 currently includes a method for the determination of unsaponifiable matter.  
3.2 The amount of unsaponifiable matter in tall oil and other related products is important in characterizing such products as it indicates the level of nonacidic material, both free and combined, present in the test material. The unsaponifiable in naval stores products is primarily composed of higher molecular weight alcohols, sterols, and hydrocarbons.
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1.1 This test method covers the determination of the percentage of material in pine chemicals products as defined in Terminology D804 including rosin, tall oil and related products, other than insoluble dirt or similar visible foreign matter that does not yield a water-soluble soap when the sample is saponified with potassium hydroxide.  
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.
Note 1: It has been reported that this method may not be applicable to gum rosin, especially any gum rosin containing volatile terpenes. Volatile terpenes are by definition unsaponifiable matter, and can be lost under the drying conditions described in 8.4. The method is applicable to tall oil rosin and wood rosin as these rosins do not contain volatile terpenes.  
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
3.1 In general, with materials of these types, softening does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results obtained are to be comparable.  
3.2 In these test methods, the softening point is defined as the temperature at which a disk of the sample held within a horizontal ring is forced downward a distance of 25.4 mm (1 in.) under the weight of a steel ball as the sample is heated at 5°C/min in a water, glycerin, silicone oil, ethylene glycol/water or glycerin/water bath.  
3.3 The automatic method was chosen to be the reference method because a round robin demonstrated that it gave more precise results than the manual method.
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1.1 These test methods are intended for determining the softening point of resins (including rosin and terpene resins) and similar materials by means of the ring-and-ball apparatus.  
Note 1: For testing asphalts, tars, and pitches, see Test Method D36.  
1.1.1 Test method using the automated ring and ball softening point apparatus is the reference method and the test method using the manual ring and ball method is an alternative method.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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
4.1 This is a revision of the method for measuring rosin acids content combines the three major ways of determining the rosin acids content of pine chemicals products into a single method.  
4.1.1 For materials containing less than 15 % rosin, the modified Glidden procedure has gained acceptance. For materials containing more than 15 % rosin the modified Wolfe Method is preferred. The modified Wolfe and modified Glidden procedures differ only in their details. They have been combined here into a single procedure. This procedure can be run using either a potentiometer or an internal indicator to determine the end point of the titration. Use of a potentiometer is preferred and is the referee method. Use of an internal indicator is the principal alternative method. They will be referred to as the Potentiometric Method and the Internal Indicator Method.
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1.1 These test methods cover the determination of rosin acids in tall oil, tall oil fatty acid, tall oil rosin, and other pine chemicals products.  
1.2 These test methods may not be applicable to adducts or derivatives of rosin, fatty acid, or other pine chemicals products.  
1.3 The values stated in SI units are to be regarded as the standard. 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
3.1 The iodine value of a fatty acid product is a measure of the unsaturated fatty acid content of that product and consequently a measure of the ease of oxidation or drying capacity of that fatty acid product.  
3.2 This test method measures the unsaturation as iodine value by addition of an iodine/chlorine reagent. The amount of reagent absorbed is determined by back titrating the excess reagent and comparing it to a blank determination.  
3.3 In samples containing conjugated double bonds, the iodine value obtained is empirical since the reagent does not react stoichiometrically with conjugated unsaturation. Where no conjugation is present, the iodine value obtained is a measure of the total unsaturation. By using proper specimen weights, the empirical values obtained are useful for comparative purposes.  
3.4 This test method was developed in order to replace the hazardous solvent, carbon tetrachloride, used in Test Method D1959 with the less hazardous and more available solvents, iso-octane and cyclohexane. As data on the satisfactory use of other solvents becomes available, this test method will be amended to include those solvents.  
3.5 This test method should have applicability to fatty acids and oils other than tall oil fatty acid but that possibility has not been investigated.
SCOPE
1.1 This test method covers the Wijs procedure for determination of unsaturation (iodine value) of tall oil fatty acids.  
1.2 Iodine value is a measure of the unsaturation of oils and fatty acids and is expressed in terms of the number of centigrams of iodine per gram of sample (weight percent of absorbed iodine).  
1.3 When this test method is used to determine the iodine value of fatty acids having conjugated systems, the result is not a measure of total unsaturated, but rather is an empirical value that affords a comparison of unsaturation. Total unsaturation of conjugated systems may be measured in accordance with Test Method D1541.  
1.4 The test method described here is not reliable for tall oil fatty acids containing an appreciable quantity of rosin.  
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.6 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.  
1.7 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
3.1 The test procedures described in this standard were developed when the chief use for turpentine was as a solvent. Currently however, the chief use for turpentine (and pinenes) is as raw materials for the production of resins and synthetic organic chemicals. Thus the chemical composition of turpentines and pinenes is extremely important and tests, in addition to the ones described in these test methods, are required in order to fully characterize turpentines and pinenes. The most widely used technique for determining the chemical composition of turpentines (and pinenes) is gas chromatography (see Test Methods D6387).
SCOPE
1.1 These test methods cover procedures for sampling and testing turpentine, as defined by the Code of Federal Regulations and Terminology D804. These test methods are also used for the sampling and testing of pinenes, the major components of most turpentines.  
1.2 These test methods primarily measure the physical rather than the chemical properties of turpentines and pinenes. As turpentines and pinenes are currently used chiefly as chemical raw materials for the production of resins and synthetic organic chemicals, chemical composition is also very important. Consequently, testing the chemical composition of turpentines and pinenes by gas chromatography has displaced these test methods to a large extent. (See for example Test Methods D6387.)  
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that 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
3.1 Rosin and similar materials such as rosin derivatives often contain volatile material derived from the raw material used or formed as a result of the processing of the rosin. This volatile material can have a significant effect on the physical and chemical properties of the rosin and so a standard method for its determination is required.
SCOPE
1.1 This test method covers the determination of the volatile oil content of rosin or similar material. The oil may consist of naturally occurring terpene oil, such as heavy fractions of turpentine, resulting from incomplete distillation in the processing of the rosin, or of foreign nonterpene oil resulting from incomplete removal of mineral or coal-tar solvent used to extract the rosin from wood or still wastes. In certain cases the volatile oil could consist of decarboxylated rosin formed during the processing of the rosin.  
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
3.1 The testing procedures described in these test methods have been in use for many years and emphasize the physical properties rather than the chemical composition of dipentene. These procedures were sufficient when dipentene was used primarily as a solvent. Currently, however, dipentene finds application as a chemical raw material and a knowledge of its chemical composition is therefore important. Test Methods D6387 describe a capillary gas chromatography method which is suitable for determining both the major and minor components found in dipentene.
SCOPE
1.1 These test methods cover procedures for sampling and testing dipentene and related terpene solvents, consisting chiefly of monocyclic terpene hydrocarbons distilling above the range for turpentine.  
1.2 The procedures given in these test methods appear in the following order:    
Section  
Sampling  
4  
Detection and Removal of Separated Water  
5  
Appearance  
6  
Color  
7  
Odor  
8  
Specific Gravity  
9  
Refractive Index  
10  
Composition  
11  
Flash Point  
12  
Moisture  
13  
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
4.1 In general, with materials of these types, softening point does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results obtained are to be comparable.
SCOPE
1.1 This test method covers the determination of softening point of resins using a Mettler cup and ball apparatus, and may, under user-defined conditions, give results comparable to those obtained by Test Methods E28.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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 This test method is used to measure the apparent viscosity of hydrocarbon resins at elevated temperatures. Elevated temperature viscosity values of a hydrocarbon resin may be related to the properties of coatings, adhesives and the like, containing such a resin.  
5.2 For hydrocarbon resins, values of apparent viscosity will usually be a function of shear rate under the conditions of test. Although the type of viscometer described in this test method operates under conditions of relatively low shear rate, shear rate depends on the spindle and rotational speed selected for a determination; therefore, comparisons between apparent viscosity values should be made only for measurements made with similar viscometers under conditions of equivalent shear rate.
SCOPE
1.1 This test method covers the determination of the apparent viscosity of hydrocarbon resins having apparent viscosities up to 2,000,000 millipascal seconds (mPa·s) (Note 1) at temperatures up to 300°C [572°F].
Note 1: The SI unit of (dynamic) viscosity is the pascal second. The centipoise (cP) is one millipascal second (mPa·s) and is frequently used as a viscosity unit.  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.  
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
3.1 Saturated fatty acids solidify at a higher temperature than unsaturated fatty acids. This test method provides a means of measuring the solidification temperature of a sample containing both unsaturated and saturated fatty acids by cooling the specimen and measuring the temperature at which solidification occurs.  
3.2 Samples containing higher levels of saturated acids will have a higher titer (solidification temperature) than those with lower levels of saturated acids.  
3.3 Water present in the sample will raise the titer, so provisions are made in the test method to remove traces of moisture.
SCOPE
1.1 This test method covers the determination of the solidification (titer) point of fatty acids and is applicable to all fatty acids.  
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
3.1 The testing procedures described in these test methods have been in use for many years and emphasize the physical properties of pine oil rather than its chemical composition. Test Methods D6387 describe a capillary gas chromatography method which is suitable for determining both the major and minor components found in pine oils.
SCOPE
1.1 These test methods cover procedures for sampling and testing pine oils, and are applicable to both natural pine oils derived from pine stumps either by the steam and solvent process or by destructive distillation, and also to synthetic pine oils obtained by the chemical hydration of terpene hydrocarbons.  
1.2 The procedures given in these test methods appear in the following order:    
Section  
Sampling  
4  
Appearance  
5  
Color  
6  
Specific Gravity  
7  
Refractive Index  
8  
Composition  
9  
Moisture  
10  
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 Thermal analysis provides a rapid method for determining transition temperatures in HC resins that possess them.  
5.2 This practice is useful for both quality assurance and research.
SCOPE
1.1 This practice covers determination of glass transition temperatures of hydrocarbon (HC) resins by differential scanning calorimetry (DSC).  
1.2 This practice is applicable to HC resins as defined in Terminology D6640. The normal operating temperature range is from the cryogenic region to approximately 180°C. The temperature range can be extended.  
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 Further discussion of glass transition can be found in Test Method D3418, and Test Method E1356.  
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.

SCOPE
1.1 Although the pine chemical industry has been a continuing producer of chemical products for many centuries, the nature of the industry, its products, and its terminology have changed. In particular, the original practice of recovering pine chemical through the processing of the exudate from pine trees has been supplemented by their extraction by solvent products of the wood pulping industry. For many years the industry was known as the Naval Stores industry but that term has gradually been replaced by the more descriptive and meaningful term, Pine Chemicals Industry. Thus, this terminology contains some old terms now mostly of historic value, together with the terms of the modern pine chemical industry.2

SIGNIFICANCE AND USE
3.1 Many pine chemical products contain water as a result of the processes used for their production. Typically refined products such as terpenes, pine oil, tall oil fatty acids, and distilled tall oil contain only traces of water, but crude tall oil might contain 0.5 to 2.5 % of water. Although the Karl Fischer and coulometric methods are most applicable to low levels of moisture, these can be and are used at higher levels. The azeotropic distillation method is generally used at higher levels.
SCOPE
1.1 These test methods cover the quantitative determination of dissolved or occluded water present in any proportion in liquid pine chemicals, such as turpentine, pinene, dipentene, pine oil, tall oil, and tall oil fatty acids. Three methods of moisture testing are included. The Karl Fisher titration method is the preferred method for testing tall oil, Test Methods D803.  
1.1.1 The Karl Fischer Titration method is based on the reaction between water and a complex reagent2 consisting of iodine, sulfur dioxide, pyridine, and methanol, whereby the iodine is converted to a colorless compound. The appearance of a persistent iodine color in the reaction mixture indicates the complete removal of free water by reaction with the reagent, and the endpoint may be measured colorimetrically. Automatic titrators find this endpoint by the restoration of a current strength when the resistance provided by the presence of water is eliminated. Amperometric automatic titrators find this endpoint by detecting the current flow that occurs once water is eliminated.  
1.1.2 The coulometric titration method determines water content by electronic integration of a current sufficient to generate the precise amount of iodine from the required reagent to react with the water in the sample.  
1.1.3 The azeotropic method utilizes the relatively low boiling point of water, as compared with other sample constituents, in a toluene or xylene matrix so that water is collected in a trap and measured.  
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.

SIGNIFICANCE AND USE
4.1 This test method provides a more precise way of measuring Gardner color than described in Test Method D1544. It is applicable to pine chemical products having colors from Gardner 1 to Gardner 18. The Gardner scale is not applicable to materials with colors lighter than 1 or darker than 18.
SCOPE
1.1 This test method covers the quantitative determination of the color of clear, yellow/brown, liquid materials using color measuring instruments. The results may be invalid if other materials are used. The test uses the Gardner color scale described in Test Method D1544. This test method applies to pine chemical products including tall oil, tall oil fatty acids, rosin, and related products.  
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, problems 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.

SIGNIFICANCE AND USE
3.1 Rosin, particularly gum and wood rosin, occasionally contains small amounts of contamination such as sand, dirt or bark. Rosin derivatives occasionally contain traces of insoluble material as a result of the raw materials used in their production or they may be generated during the production process. In all instances the presence of such insoluble material should be minimal. This test method describes a rapid and reliable procedure for determining the amount of such insoluble matter. It is based on the knowledge that rosin and most of its derivatives are soluble in numerous organic solvents whereas most common contaminants are not. It is especially useful for internal quality control rather than sales specifications.
SCOPE
1.1 This test method covers the determination of the amount of insoluble matter in rosin and rosin derivatives as described in Terminology D804.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
5.1 This practice is useful for both quality control and research.
SCOPE
1.1 This practice covers determination of the color stability of a hydrocarbon resin by exposure to a specific temperature for a defined time period in a forced-draft oven.  
1.2 Color stability is measured by the change in color of the test resin, measured via the yellowness index color scale, in accordance with Practice E313, or the procedure for Gardner Color, Test Method D6166.  
1.3 The values stated in SI units are to be regarded as standard. 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
3.1 Rosin is an important product of the centuries old Naval Stores industry, now known as the Pine Chemical industry, and is produced and consumed in many countries throughout the world. Consequently, reliable methods of sampling and grading rosin are necessary. The test methods based on the use of the USDA Official Standards described herein, were developed many years ago for the sampling and grading of rosin and are similar to those included in the Naval Stores Act.3  
3.2 Although these test methods based on the use of the USDA Official Standards are still applicable, many additional test methods are now used to grade rosin. In particular, the color of rosin is now more commonly reported using the Gardner color scale rather than the USDA Official Standards. In addition, Test Methods E28, D465, and D5974 are widely used to assess the quality of rosin in addition to the color grading methods described in this standard.
SCOPE
1.1 These test methods cover procedures for sampling and determining the grade of rosin delivered in commercial bags, barrels, drums or in molten form. Although developed for rosin, these methods can also be used for the grading of modified rosins and rosin based resins.
Note 1: All rosin sold in interstate commerce must be described by reference to the U. S. Standards for rosin, and is therefore subject to grading prior to such sale. The grading procedure described in these test methods is used for checking grades or regrading after the rosin has moved from the primary markets to distributing or consuming points.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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.

SIGNIFICANCE AND USE
4.1 These test methods are designed to broaden the scope of the previous edition of these test methods by the inclusion of tall oil as a test material. Test Methods D803 currently includes methods for the determination of the rosin acid and fatty acid content of crude tall oil. Test Methods D803 references Test Method D1585.  
4.2 Rosin and tall oil are composed primarily of rosin acids and fatty acids, and the measurement of these components is important in establishing the composition of these materials.
SCOPE
1.1 These test methods cover the determination of the fatty acids of pine chemicals, including rosin, tall oil, and related products.  
1.2 These test methods may not be applicable to adducts or derivatives of rosin or other pine chemical products.  
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.

SIGNIFICANCE AND USE
4.1 For hydrocarbon resins and rosin based resins, softening does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle solids or very viscous liquids to less viscous liquids. For this reason, determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results obtained are to be comparable.
SCOPE
1.1 These test methods are intended for determining the softening point of hydrocarbon resins, rosin based resins and similar materials by means of an automated ring-and-ball apparatus. Portions are similar in technical content to the automated-apparatus versions of Test Methods D36, E28, and ISO 4625.  
1.1.1 The ring-and-ball softening point of a hydrocarbon resin and rosin based resins may also be determined with lower precision using the manual ring-and-ball softening point procedure in Test Methods E28.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 This standard method 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.

SIGNIFICANCE AND USE
3.1 These test methods are designed to broaden the scope of the earlier editions of the test method by the inclusion of tall oil and tall oil derived products as test materials and will be referenced in Test Methods D803.  
3.2 The acid number is an important property of pine chemical products, such as tall oil, and the products obtained by the fractionation of tall oil. It is the test method widely used to determine the total free acid content of these products.  
3.3 The potentiometric test method should be used when the most reproducible results are required.
SCOPE
1.1 These test methods are intended for determining the acid number of pine chemical products as defined in Terminology D804 including tall oil products, wood and gum rosin, and other related materials. These test methods may not be applicable to all modified rosin products. Two test methods are covered, as follows:  
1.1.1 Potentiometric method (referee), and  
1.1.2 Internal indicator method (alternate).  
1.2 The potentiometric method is suitable for use with both light- and dark-colored products. It should be considered the referee method. The internal indicator method is suitable for use only with light- and medium-colored products with a Gardner color of less than 12. It should be considered the alternate method.  
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 and health practices and determine the applicability of regulatory limitations prior to use.